US2761791A - Method of multiple coating - Google Patents

Method of multiple coating Download PDF

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Publication number
US2761791A
US2761791A US489863A US48986355A US2761791A US 2761791 A US2761791 A US 2761791A US 489863 A US489863 A US 489863A US 48986355 A US48986355 A US 48986355A US 2761791 A US2761791 A US 2761791A
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United States
Prior art keywords
coating
layers
bead
support
solutions
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.)
Expired - Lifetime
Application number
US489863A
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English (en)
Inventor
Theodore A Russell
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.)
Eastman Kodak Co
Original Assignee
Eastman Kodak 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
Priority to CA557259A priority Critical patent/CA557259A/en
Priority to CA557260A priority patent/CA557260A/en
Priority to CA557258A priority patent/CA557258A/en
Priority to IT557307D priority patent/IT557307A/it
Priority to CA554506A priority patent/CA554506A/en
Priority to BE545464D priority patent/BE545464A/xx
Priority to US489969A priority patent/US2761419A/en
Application filed by Eastman Kodak Co filed Critical Eastman Kodak Co
Priority to US489862A priority patent/US2761418A/en
Priority to US489861A priority patent/US2761417A/en
Priority to US489863A priority patent/US2761791A/en
Priority to DEE11998A priority patent/DE1211488B/de
Priority to DEE11997A priority patent/DE1216686B/de
Priority to DEE11996A priority patent/DE1208998B/de
Priority to DEE11995A priority patent/DE1151173B/de
Priority to FR1148817D priority patent/FR1148817A/fr
Priority to GB26305/59A priority patent/GB834527A/en
Priority to GB5590/56A priority patent/GB834525A/en
Priority to GB26306/59A priority patent/GB834528A/en
Application granted granted Critical
Publication of US2761791A publication Critical patent/US2761791A/en
Priority to US769881A priority patent/US2975754A/en
Priority to DEE18311A priority patent/DE1177931B/de
Priority to FR808185A priority patent/FR1238160A/fr
Priority to GB36130/59A priority patent/GB901686A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D1/00—Processes for applying liquids or other fluent materials
    • B05D1/34—Applying different liquids or other fluent materials simultaneously
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C—APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C5/00—Apparatus in which liquid or other fluent material is projected, poured or allowed to flow on to the surface of the work
    • B05C5/007—Slide-hopper coaters, i.e. apparatus in which the liquid or other fluent material flows freely on an inclined surface before contacting the work
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C—APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C5/00—Apparatus in which liquid or other fluent material is projected, poured or allowed to flow on to the surface of the work
    • B05C5/02—Apparatus in which liquid or other fluent material is projected, poured or allowed to flow on to the surface of the work the liquid or other fluent material being discharged through an outlet orifice by pressure, e.g. from an outlet device in contact or almost in contact, with the work
    • B05C5/0254—Coating heads with slot-shaped outlet
    • B05C5/0258—Coating heads with slot-shaped outlet flow controlled, e.g. by a valve
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C—APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C9/00—Apparatus or plant for applying liquid or other fluent material to surfaces by means not covered by any preceding group, or in which the means of applying the liquid or other fluent material is not important
    • B05C9/06—Apparatus or plant for applying liquid or other fluent material to surfaces by means not covered by any preceding group, or in which the means of applying the liquid or other fluent material is not important for applying two different liquids or other fluent materials, or the same liquid or other fluent material twice, to the same side of the work
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/07—Flat, e.g. panels
    • B29C48/08—Flat, e.g. panels flexible, e.g. films
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/16—Articles comprising two or more components, e.g. co-extruded layers
    • B29C48/18—Articles comprising two or more components, e.g. co-extruded layers the components being layers
    • B29C48/21—Articles comprising two or more components, e.g. co-extruded layers the components being layers the layers being joined at their surfaces
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/255—Flow control means, e.g. valves
    • B29C48/2556—Flow control means, e.g. valves provided in or in the proximity of dies
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/30—Extrusion nozzles or dies
    • B29C48/305—Extrusion nozzles or dies having a wide opening, e.g. for forming sheets
    • B29C48/307—Extrusion nozzles or dies having a wide opening, e.g. for forming sheets specially adapted for bringing together components, e.g. melts within the die
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/30—Extrusion nozzles or dies
    • B29C48/305—Extrusion nozzles or dies having a wide opening, e.g. for forming sheets
    • B29C48/31—Extrusion nozzles or dies having a wide opening, e.g. for forming sheets being adjustable, i.e. having adjustable exit sections
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/88—Thermal treatment of the stream of extruded material, e.g. cooling
    • B29C48/911—Cooling
    • B29C48/9135—Cooling of flat articles, e.g. using specially adapted supporting means
    • B29C48/914—Cooling of flat articles, e.g. using specially adapted supporting means cooling drums
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B11/00—Treatment of selected parts of textile materials, e.g. partial dyeing
    • D06B11/0056—Treatment of selected parts of textile materials, e.g. partial dyeing of fabrics
    • D06B11/0069—Treatment of selected parts of textile materials, e.g. partial dyeing of fabrics by continuous contact with a member able to bring simultaneously a plurality of treating materials
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H23/00—Processes or apparatus for adding material to the pulp or to the paper
    • D21H23/02—Processes or apparatus for adding material to the pulp or to the paper characterised by the manner in which substances are added
    • D21H23/22—Addition to the formed paper
    • D21H23/46—Pouring or allowing the fluid to flow in a continuous stream on to the surface, the entire stream being carried away by the paper
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H5/00—Special paper or cardboard not otherwise provided for
    • D21H5/0005—Processes or apparatus specially adapted for applying liquids or other fluent materials to finished paper or board, e.g. impregnating, coating
    • D21H5/0042—Processes or apparatus specially adapted for applying liquids or other fluent materials to finished paper or board, e.g. impregnating, coating by pouring or allowing to flow in a continuous stream onto the surface, the entire stream being carried away by the paper
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03C—PHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
    • G03C1/00—Photosensitive materials
    • G03C1/74—Applying photosensitive compositions to the base; Drying processes therefor

Definitions

  • the present invention relates to a method of applying a plurality of separate coating materials to a support in layer relationship, and particularly to a method of applying all of the coating materials simultaneously while maintaining a distinct relationship between the different layers after they have been cured or dried on said support.
  • the final product consists of a support having a plurality of distinct layers of the coating materials on one surface thereof.
  • the different layers of coating will have different individual functions in the final product and it is, therefore, necessary that the individual coatings remain distinct from one another, i. e. that one layer not contaminate nor mix with the adjacent layer and that each layer have a given thickness which may or may not be the same as the thickness of any of the other layers.
  • a classic example of such a multiply coated support is found in the manufacture of photographic films and papers.
  • a simple photographic film may consist of a support of some cellulose derivative, i. e. cellulose acetate, which has coated on one surface thereof a lightsensitive emulsion and on top of that a coating of some transparent material whose function it is to protect the emulsion from abrasion.
  • Such a film may also have a thin subcoat of some material applied to it before emulsion coating in order to facilitate spreading of the emulsion thereon and to increase its tenacity with the support.
  • the colors sensitive photographic films then there are several individual coatings which must be applied. There may be the subcoating, a blue sensitive emulsion, a red-sensitive emulsion, a green-sensitive emulsion, a protective coating, one or more color filtering coatings, etc.
  • each layer is identical and contamination or mixing between layers is not a factor. Or, stating it another Way, there is no necessity for keeping the individual layers distinct from one another.
  • One object of the present invention is to provide a method of applying a plurality of separate coating materials to a support simultaneously and still maintain a distinct relationship between the different layers.
  • Another object is to provide a method of coating a support with a plurality of coating materials simultaneously and curing or drying all of said layers at the-same time while still maintaining a distinct layer relationship between the coatings.
  • a further object is to provide a method of coating as described which involves the customary bead method of coating, but in which the several coating materials are simultaneously fed into said bead and are coated therefrom in the desired layer relationship.
  • Yet another object of the present invention is to provide a method of coating a plurality of colloidal-materials onto a support in distinct layer relationship which comprises simultaneously applying each of the colloidal materials in solution form onto the support at the same point.
  • Still another object is to provide a method of coating a support in the manufacture of photographic film and/or paper which comprises simultaneously applying one or more light-sensitive emulsions, and/ or subcoatings, protecting layers and light filtering layers to the support at the same time and maintaining a distinct layer relationship as well as a desired thickness regulation of each layer.
  • Fig. 1 is a schematic, part side elevational, part sectional, view of'a form of apparatus including a dual hopper which may be used to simultaneously apply two layers of coating material to a web in accordance with the present invention
  • Fig. 2 is an enlarged sectional view of just the dual hopper used in connection with the apparatus of Fig. 1;
  • Fig. 3 is a greatly enlarged fragmentary section of the dual hopper shown in Fig. 2 and illustrating how two layers of coating material are simultaneously applied to the surface of a web;
  • Fig. 4 is a fragmentary section showing a color photographic film coated with four difierent layers of material and using a dual hopper;
  • Fig. 5 is an enlarged fragmentary section of a triple hopper by the use of which three layers of coating material may be applied to a surface of a web in accordance with the present invention
  • Fig. 6 is a front elevational view of a multiple hopper which can be used to simultaneously apply four coatings to the surface of a web in accordance with the present invention
  • Fig. 7 is a partial top plan view of the multiple hopper shown in Fig. 6;
  • Fig. 8 is a sectional view taken substantially on line 88 of Fig. 6;
  • Fig. 8A is an enlarged detail of Fig. 8 showing how' 5 into the coating bead by the hopper;
  • v Fig. 9 is a "sectional view of a dual slide hopper by. means of which'two layers of coating material may be simultaneously applied to the surface of a web in accordance with thepresent invention
  • Fig. l0 is a sectional view-of :a multiple slide lhopper b y .the use of which four layers of coating. material may be applied to the. surface of a web simultaneously in accordance with the .present invention;
  • Fig. 11 is-a sectional view showing a combined-extrusion and'slide hopper by means of which two layers of coating material may be simultaneously applied to a surface of a web in'accordance with 'thepresent invention
  • V V a Fig-l2 is a sectional view showing --a combined-extrusion and slidehopper by means of whiehithreie layers of coating material may be appliedr-imaccordance with the :present invention.
  • the customary'*p'r6cedureof applyingth'esecoatirigs has been to applythem one at'a time in succession "and' 'setting and drying each coating before applyingthe succeeding one.
  • These coatings are "usually ⁇ applied by putting the diflei'ent materials in solution and coating them in this form, by any number of difierent't'echn'iques; onto-a 'con-'' tinuously moving support.
  • the present invention is concerned with the discovery that' two' or inore'of'these coatings can be'app'lied to a support simultaneously and still maintain"a"di'stin ct relationship "between the layers.
  • The" difiere'nt materials coated according to the present invention althou'gh 'co'at'ed in' the form "of solutions, do'n'ot"'-show anymorecontamination or mixture 'at' the interface" ofthe lawman-an the same materials when' coatedin successiodbythe ens- Inthe case of color films -these separ'ate-coating's mayinclude three separate silver-halide avenger tomary technique which involves a .completesettingand drying of each coat before the next is applied.
  • this novel method of coating the desired individual thickness of each layer of coating material can be regulated to the same extent as when the coatings are applied separately. Furthermore, this method is particularly suitable for applying thin coatings, or coatings having a dry thickness of fro'm..'less than one micron to 105025 inch.
  • This phenomenon is not limited to the coating of difcoatings of a photographic film, since each of the separate coatings in such a product are essentially waterpermeable gelatin solutions difiering only in the silver salt, the dye, or other materials, suspended or dispersed therein.
  • his desirable ⁇ to include .a. coating .aid such 'as isaponi-n, an ialkylisnlfate,
  • this methodv of coating involves putting the materials to becoated in solution and simuL;
  • coatingtapparatususoglong.asiit permits the formation of each? ofzzthe' coating compositions "into i a layer of "dc-1 sired-zithickness-zand tthenapermitsythese layers to :be
  • the layer of coating solutiondeaving the dating: device instead 0f (:o'atirlg -directly ioutaontotheweb in a layer-having a'thickness zequal to thatzleaving- .5 side of the coating device from which the web departs.
  • This pile up or puddle of coating solution extends completely across the width of the web being coated and is normally referred to as a bead of coating.
  • An enlarged cross-section of a typical coating bead is shown at 17 in Fig. 3. It can thus be seen that with this bead coating technique the coating is not in fact deposited directly onto the web from the coating device, but the coating device merely maintains the coating bead and the web is coated therefrom.
  • the thickness of the coating laid down on a web moved thereacross will be determined by the action of the bead and will vary with the speed of web movement, the rate of supply of the coating solution, etc., and will not necessarily be equal to the width of the exit slot of the coating device.
  • coating bead will be used to mean a puddle or pile up of coating solution maintained in bridging relation between the surface of a web to be coated and a coating device which is stationary relative to the head of coating and spaced transversely from the support and across and in contact with which the surface of a web is moved to be coated therefrom.
  • the term bead coating will refer to that method of coating a web where the surface thereof is moved across and in contact with a coating bead and takes up the coating therefrom.
  • Figs. 1 and 2 there is shown an apparatus which was successfully used to prove that this principle of coating at least two layers simultaneously onto a support was sound.
  • a dual-feed coating hopper 10 having an exit slot 11, the lips 12 of which are slightly spaced from the surface of a web W backed up by a roll 13 which may serve to continuously move the web past the hopper slot.
  • One coating solution S is continuously fed into an upper inlet 14 by a suitable metering pump P
  • the second coating solution S is continuously fed into the lower inlet 15 by a separate metering pump P, see Fig. 2.
  • An adjustable baffle 16 divides the interior of the hopper into two separate cavities and serves to direct the two solutions in the form of thin layers L and L toward the hopper slot 11.
  • the hopper was made of a transparent plastic material and differently colored coating solutions were used so that the behavior of the solutions could be watched and it was obvious that the layer L of solution S coming into the upper inlet was on top of the layer L of the solution S coming into the lower inlet throughout the entire length of the exit slot 11.
  • This distinct layer relationship was maintained in the bead, despite apparent deformation of the bead, and an enlarged cross-section of the coated web after being dried showed that the two layers were distinct, extremely free of contamination or mixing at their interface, and possessed a relative thickness comparable to the rate at which each solution was pumped into the hopper.
  • the hopper 10 may be provided with any suitable form of adjustable mount so that the position of its exit slot 11 relative to the surface of the web W being coated can be adjusted for the best coating procedure.
  • the hopper is carried by a frame 18 provided with bearings 9 rotatably journalled on the axle 8 of the backing roll 13 to permit the mount to be swung concentrically of the backing roll 13 so that the position of the hopper as a whole may be shifted around said roll.
  • the frame 18 is capable of being locked in any adjusted position by means of a clamping screw 7 engaging an arcuate slot 6 in the support 19.
  • the hopper per se is pivoted to the frame 18 at 29 so that the angle of the exit slot 11 may be critically adjusted relative to the surface of the web to be coated by means of adjustment of screw 5.
  • the hopper is slidably mounted on the frame 18 and connected with an adjusting screw. 21.
  • the coatings ap-. plied may be of the type which are set by cooling prior Referring to Figs. 2 and 3, it will be seen that the coating composition S entering upper inlet 14 is formed into a layer upon passing between the end of the bathe 16 and the upper inclined wall 24 of the hopper.
  • the coating composition S entering the lower inlet 15 is formed into a layer upon passing between theend of this baflie 16 and the lower inclined wall 25 of the hopper. These two layers are then brought into surface contact just prior to, or upon, entering the exit slot 11 of the hopper and are then directed by this hopper in this combined relation into the coating head 17 wherein they maintain the desired distinct layer relationship, as indicated in Fig. 3, and from which bead the layers are simultaneously coated on the surface of the web inthe desired layer relationship.
  • the width of the exit slot 11 is not equal to the combined thickness of the layers of coating composition directed thereto, but is preferably equal to the thickness of one of said layers or may even be less than this. This means that the velocity of the combined layers L and L passingthrough the exit slot 11 must be greater than that of the individual layers as they approach the slot, i. e. double,
  • the relative widths of the exit slot 11 and the slots forming the individual layers of the diiferent coating compositions must be such as to permit the proper amount of the different solutions to be fed to the bead as determined by the bead laydown, and the rate at which the difierent compositions are pumped will be determined by the relative thickness of the two layers desired on the web. For example, if the coating S applied is to be twice as thick as coating S, then the slot widths are not varied, but coating S is pumped into the hopper at a rate twice that of coating S.
  • the colored gelatin was pumped into the hopper through the upper inlet 14 by a metering pump from a solution containing about seven percent dry gelatin. Both pumps were driven simultaneously with a commercial metering unit. Two coatings were made on a cellulose acetate support, one at twelve feet per minute and the other at eighteen feet per minute and in each case the two layers were simultaneouslyjset'and dried by conventional equipment. Enlarged fcIOSS-seCtiOns of "the dried"films-showed excelle'nt' separation of the gelatin *and light-sensitive emulsio'n layers, and indicated that the relative thickness of the two "coatings was directly proportional 'to "the-rate at which the different solutions were pumped into the hopper.
  • this coated product comprises asupportor web W of cellulose acetate having successive layersof a blue-sensitized silver chlorobromide emulsion- B, ared-sensitized silver chlorobromide emulsion R, a green sensitized silver chl'orobromide emulsion G and a clear gelatin layer C, in that order. Since onlya dualfeed-hopper was used, the first two emulsions R andB wereapplied simultaneously. and the .third emulsion andandwas coated .at the rate of 21.30 pounds per silver moleand 1.78 pounds per hundredsquare feet giving a coverage of 1200 square feet per silver mole.
  • a triple feed hopper of the type shown in Fig. 5 was constructed.
  • This hopper 26 has an'exit slot 30, the lips 32 of which are slightly spaced from the surface of a web Whacked by'a roll 13'which may serve to continuously move the web past thehopper slot as before.
  • the coa ing' material S" which is to be the bottom layer L" was pumped into the lower inlet 33, the coating material S which-was to be the center layer L was fed into the intermediate inlet 34, and the coating material S which was to be the top layer L was fed into the top inlet 35.
  • Thethree coating materials were then directed to ward the hopper exit slot '30 by layer forming slots 36, 37*and 38, respectively, andthe three layersformed uponpassage through these slots flowed in combined relation through said exit-slotiati in theproper striated relationship.
  • This triple feed hopper was tested in makingithe'lfour layer experimental;color .print' coating described" above.
  • the blue; red, and green-sensitive emulsions were applied simultaneously .as superposed liquidlayers in .the order specified and at a'coating speed of approximately twelvefeet per minute.
  • the emulsions were set and dried simultaneously :by means of apparatus substantially like that disclosedrin Fig. l, and the cleargelatin overcoatwas vappliedseparatelyandset and dried.
  • a check coatingwastthen made of these same materials by coating eachmaterial individually in the conventional-manner.
  • a four-tube, multifeed hopper of the type shown in Figs. 6-8 was constructed and it was determined that four different coating materials could be simultaneously applied to a web and still maintain a distinct layer relationship between the coatings.
  • This hopper is composed of a top section 40 and a bottom section 41 which are held in assembled relation by two end plates 42 and 43 fastened to the top and bottom sections by bolts 44.
  • the forward edges of each of the top and bottom sections are spaced from one another to provide an exit or discharge slot 45 which extends across the width of the hopper and whose width is defined by end plates 42 and 43.
  • the bottom section 41 is provided with a recess or chamber 46 communicating with the exit slot of the hopper by a curved convex surface 47.
  • This chamber is divided into four sections by three dams 48, 49 and 50 which extend entirely across the width of the hopper chamber 46.
  • Each of these dams includes a concave curved surface 51 and a convex curved surface 52 which cooperate with one another in opposite pairs to form gradually restricted flow passages 53, 54, 55 and 56 which cause coating solutions pumped into the enlarged portions thereof to spread out across the hopper and to be forced in thin streams or layers toward the hopper discharge slot 45.
  • each of the dams 48, 49 and 50 is made adjustable by means of a pair of adjusting screws 62 and set screws 63.
  • each of the discharge slots 59, 60 and 61 can be regulated to the desired extent, and after the desired adjustment has been made, the set screws 63 are adjusted to lock the dams in such positions.
  • Each of the four flow passages has connected thereto a nipple 64 onto the end of which one of four feed tubes 65, 66, 67 or 68 may he slipped.
  • Each of the four feed tubes is connected to a supply of a different coating solution and from which supply the coating solution can be pumped into the hopper by separate metering pumps P at rates commensurate with the thickness of the particular coating layers desired in the final laydown.
  • the relative thicknesses of the individual layers of the difierent coating solutions deposited on the web W will depend not upon the width of the discharge slot formed by the several dams and the upper section of the hopper but will depend upon the rate at which the respective coating compositions are pumped into the hopper. I have found that the above-mentioned orientation of the different layers of coating solution will not be affected by the order in which the pumping of the different solutions into the hopper is started.
  • This four-tube multifeed hopper was tested and proved by making a multiple coating of black and clear gelatin on a web of photographic support in the following manner.
  • the black gelatin was prepared by dispersing 2450 grams of a 3.7 percent black gelatin con taining a metallic silver dispersion in 5500 grams of ten percent photographic gelatin plus 1070 cc. of distilled water.
  • the clear gelatin coatings were made from a solution of 6810 grams of ten percent photographic gelatin plus 2850 cc. of distilled water. Twenty cc. per liter of a 7 /2 percent saponin solution were added to each coating solution to act as a coating aid.
  • the coatings were made by applying the black gelatin in the first and third layers and the clear gelatin in the second and fourth layers. With the hopper shown in Figs. 68, this meant feeding the black gelatin into feed tubes 65 and 67 and the clear gelatin into feed tubes 66 and 68 and running the web W in a counterclockwise direction as indicated. After these coatings were set and dried, a photomicrograph of a cross-section of the multiple coating showed that all of the coats applied satisfactorily and that each layer was oriented in the proper relation. Furthermore, there appeared to be no mixing or contamination of the individual layers.
  • Two polyvinyl alcohol solutions one a polyvinyl alcohol light-sensitive emulsion and the other a clear polyvinyl alcohol solution, were prepared and coated on a polyvinyl alcohol subbed cellulose acetate support at approximately twelve t'eet per minute.
  • the triple feed hopper shown in Fig. 5 was used in this test with one of the chambers blanked out so that only two layers could be coated simultaneonus'ly.
  • the clear polyvinyl alcohol solution was a six percent clear polyvinyl alcohol solution containing 95 cc. 7 /2 percent saponin solution and 250 cc. four percent borax solution per pound of polyvinyl alcohol.
  • the lightsensitive solution was coated directly on the support at 3.0 pounds per hundred square feet and this was overcoated with l.5pounds per hundred square feet with the clear polyvinyl alcohol solution. After coating, these layers of coating material were set at room temperature by fuming with ammonia as described in U. S. Patent No. 2,376,371. Cross-sections were made of this coating, and under the microscope two distinct layers were visible and no apparent mixing of the two layers appeared to have occurred.
  • the'top coat consisted'ofa'seven'percent gelatin solution containing a yellow colloidal silver dispersion and 270'cc.'of a seven and one-half'percent'saponin solutionfperp'ound of gelatin.
  • the middle coat consisted of a"'seven "percent' gelatin "solution containing 63 cc. of a seven and one-half percent 'saponin solution'per pound of :gelatin.
  • thc'ethyl cellulosephthalate employed as a coating composition wasiin thefor'rnot its salt, such as ammonium'salt, which-is" water soluble and two layers of this material were applied, according to this invention, onto acellulose'acetate'support with a coverage'of L25 poundsper hundred square feet *and' at al coating speed of six feet per minute.
  • the top layer was coated'froma clear solution "ofcellulose "'ether'phthalate saltand the bottom layer contained one part of carbon dispersion (Aqua Blak, made 'by -BinneyGmith) to nine parts'of the cellulose ether phthalate.
  • the .carbon dispersion' was' added to one of the coatingcompositions merely to show whether or not the two'materials coated in distinct layer relationship without contamination or mixing" at the interface of the layers. Photornicrographs of a' cross-section of the webso coated showed clearly that good separation of the layers was also obtained with these coating compositions.
  • This novel method of multiple coating a web is not limited to the use of extrusion type hoppers alreadydisclosed, but can be successively carried out, even with certain advantages, with other types ofcoating devices.
  • This method of coating may be readily carried out by the use of a multiple slioehopper of'the type'disclosed in jcopending US. application Serial No. 489,969,.filed on even date herewith in the names. of MercierQT-l-orpey and Russell.
  • FIG. 9 there is shown a double slide hopper by the use of which adu'al coating may be made in accordance with the present invention.
  • one 'fiuid coating composition '74 is continuously pumped by a metering pump'P into a cavity '75 at a given rate throu'gti.inlet 7otandflfrom which itis'torced through a narrow vertical .slot77 .in.the term of a ribbon and out onto a downwardly inclined slide surface"-78 down which it 'flows by gravity in the form of a'layer"79 'to a point where it forms a coating head 17 between the end of the slide surface anda web' W moved upwardly across and in contact Withfthe' beadby .a supporting roll 13.
  • the second coating composition 80 is continuously pumpedinto a second cavity 31 at a ,given rate by another'meteringpump'P through inlet 82 and from which it is forced through a narrow vertical slide83 in'the form of a ribbon and onto a second-downwardly inclined slide surface8 4. Thishribbon of the second coatingcomposh tion inifiowingdown the slide. surface 84 under the influenceof gravity forms aismoo'th,'uniformly'thiclnlayer 85. The twouslide.
  • sni-faces '78iand 84 are co'planar, or substantially so, so .thatas the layer-"diofthe second coatingcomposition reaches the ribbon of thefirst coating composition .being extruded through slot7"7, it"flows up -ontop of..the sarneoand the two then flow -to-' gether. downslide surfaceVS and into the coating head 17.
  • Fig. there is shown a l our slide hopper by the use of which four separate layers of the same or different coating compositions can be simultaneously applied to the surface of a web in accordance with the present invention.
  • the first coating composition is continuously pumped at a given rate into a cavity 90 from which it is extruded through a narrow vertical slot 91 out onto a downwardly inclined slide surface 92 over which it flows by gravity to form a layer of that compo-sition.
  • other coating compositions are continuously pumped into chambers 93, 94 and 95 and are extruded from narrow vertical slots 96, 97 and 98 respectively onto slide surfaces 99, 100 and 101, respectively, down which they flow by gravity to form separate layers of the different compositions.
  • the four slide surfaces are coplanar so that as the layers of difierent coating compositions flow down their respective slide surfaces they are brought together in overlapping relation and by the time the four layers reach the coating head 17 they are combined in the desired laminated relationship.
  • This distinct layer relationship is maintained throughout the bead so that as the Web W is moved across and in contact with the head, it takes up on its surface the four layers of coating in the desired orientation and with the layers being distinctly separate from one another and of a relative thickness commensurate with the rate at which each was pumped into the hopper. So far as I have been able to ascertain, there is no limit as to the number of separate layers of coating compositions which can be laid down on a Web with a multiple slide hopper of this type.
  • This method of multiple layer coating is not limited to the use of hoppers of the extrusion type or of the slide hopper type but is equally adapted to the use of a combination of these two types of hoppers which are disclosed in copending U. S. application Serial No. 489,864, filed on even date herewith in the names of Wilson, Sanford and Russell.
  • a hopper which combines a single slide hopper with a single extrusion hopper in accordance with the Wilson et al. disclosure.
  • one fluid coating composition X is continuously pumped into a chamber 110 and is extruded therefrom as a layer 111 from a substantially horizontal extrusion slot 112 directly toward the coating bead 17 across and in contact with which the web W is moved in the direction of the arrow while passing around roll 13.
  • the other coating composition Y is continuously pumped into chamber 113 at a given rate and is extruded as a ribbon through substantially horizontal slot 114 onto a downwardly inclined surface 115.
  • this ribbon of solution flows down the slide surface 115 by gravity, it is formed into a layer 116 of desired thickness and is brought into surface contact with the layer 111 of the other coating composition at the time it leaves extrusion slot 112 so that they move into the coating bead in combined relation.
  • these two layers of coating composition are picked up by the Web W and appear on the web, after drying, as two separate and distinct layers oriented so that the layer 111 extruded through slot 112 lies directly on the surface of the web and the layer 116 formed on the slide surface lies on top of layer 111.
  • a hopper which combines a single slide hopper with two extrusion hoppers in accordance with the Wilson et al. disclosure, and by the use of which a triple coating can be made on a web in accordance with thepresent invention.
  • one coating solution Z is continuously pumped into a chamber 120 and is extruded as a layer 121 from an upwardly inclined slot 122 directly toward the coating bead 17" across and in contact with which the surface of a web W is moved in the direction of the arrow while passing around backing roll 13.
  • a second coating solution Z' is continuously pumped into chamber 123 at a known rate and is extruded as a layer 124 from a substantially horizontal slot 125 directly toward the coating head.
  • the third coating solution Z" is continuously pumped at a known rate into chamber 126 and is extruded as a ribbon through a substantially horizontal slot 127 onto a downwardly inclined slide surface 128. As this ribbon of solution flows down the slide surface 121, it is formed into a layer 129 of desired thickness and smoothness. It will be observed that the extrusion slots 122 and 125, and the lower end of the slide surface 128, are so disposed that the three layers of coating solution formed individually thereby or thereon, as the case may be, are brought together in surface contact with one another just prior to the three layers entering the coating bead and prior to being applied to the web.
  • each hopper charnber has its own extrusion or distributing slot (122 and 125) so that the layers of the individual coating solutions do not meet until after passing from the slots.
  • the elementof time might be the critical factor since thev time elapsing between the deposition of the layers on the web and the time 'thecoating is dried is relatively shortv and perhaps less'than the time required for the coatings, or the materials dispersed therein, to diifuse into one another.
  • the coating at the tllIlEDf application is in liquid condition, and in order to accomplish drying of that coating,it may be desirable that ltfirst be set.
  • One way of doingthis is chemically, as taught by U. S. Patent 2,652,345, which teaches adding an. aldehyde to thecoating solution and 'then fuming the same after coating with gaseous ammonia to rapidly-set the coating.
  • the method of simultaneously applying thin coatings of a plurality of colloi'dalmaterials onto a Web support in distinct layer relationship comprising the steps of making a solution of each of said colloidal materials, forming a coating head of said solutions in bridging relation between the surfaceof the support and a stationary coating device spaced transversely therefrom, simultaneously feeding each of said solutions in the form of a layer into said head and in superposed relation to'i'the other solutions whereby "the individual layers are maintained in distinct superposed relation, and continuously moving the surface of said support across and in contact with said bead so that the surface of the support engages one of the outermost of the superposed layers in said head and simultaneously picks up all of said layers and moves away from the head with the solutions in distinct superposed layers.
  • the method of simultaneously applying thin coatings of a plurality of polyvinyl alcohol solutions onto a web support in distinct layer relationship comprising the steps of forming a coating head of said solutions in bridging relation between the surface of the support and a stationary coating device spaced transversely therefrom, simultaneously feeding each of said solutions in the form of a layer into said bead and in superposed relation to the other solutions whereby the individual layers are maintained in distinct superposed relation, and continuously moving the surface of said support across and in contact with said bead so that the surface of the support engages one of the outermost of the superposed layers and moves away from the head with the solutions in distinct superposed layers.
  • the method of simultaneously applying thin coatings of a plurality of gelatin and polyvinyl alcohol solutions onto a web support in distinct layer relationship comprising the steps of forming a coating head of said solutions in bridging relation between the surface of the support and a stationary coating device spaced transversely therefrom, simultaneously feeding each of said solutions in the form of a layer into said head and in superposed relation to the other solutions whereby the individual layers are maintained in distinct superposed relation, and continuously moving the surface of said support across and in contact with said head so that the surface of the support engages one of the outermost of the superposed layers in said bead and simultaneously picks up all of said layers and moves away from the head with the solutions in distinct superposed layers.
  • the method of simultaneously applying thin coatings of a plurality of liquid gelatino silver halide emulsions onto a web support in distinct layer relationship comprising the steps of forming a coating bead of said emulsions in bridging relation between the surface of the support and a stationary coating device spaced transversely therefrom, simultaneously feeding each of said emulsions in the form of a layer into said head and in superposed relation to the other emulsions whereby the individual layers are maintained in distinct superposed relation, and continuously moving the surface of said support across and in contact with said bead so that the surface of the support engages one of the outermost of the superposed layers in said bead and simultaneously picks up all of said layers and moves away from the head with the emulsions in distinct superposed layers.
  • the method of simultaneously coating a gelatin solution and a liquid gelatino silver halide emulsion onto a web support in distinct layer relationship comprising the steps of forming a coating head of said solution and emulsion in bridging relation between the surface of the support and a stationary coating device spaced transversely therefrom, simultaneously feeding each of said gelatin solution and said emulsion in the form of a layer into said bead and in superposed relation with each other whereby the individual layers are maintained in distinct superposed relation, and continuously moving the surface of said support across and in contact with said bead so that the surface of the support engages one of the superposed layers in said head and simultaneously picks up each of said layers and moves away from the bead with the gelatin solution and gelatino silver halide emulsion in distinct superposed layers.
  • the method of simultaneously applying thin coatings of a plurality of polyvinyl alcohol silver halide solutions onto a web support in distinct layer relationship comprising the steps of forming a coating head of said solutions in bridging relation between the surface of the support and a stationary coating device spaced transversely therefrom, simultaneously feeding each of said solutions in the form of a layer into said head and in superposed relation to the other solutions whereby the individual layers are maintained in distinct superposed relation, and continuously moving the surface of said support across and in contact'with said head so that the surface of the support engages one of the outermost of the superposed layers in said head and simultaneously picks up all of said layers and moves away from the head with the solutions in distinct superposed layers.
  • the method of simultaneously coating a liquid gelatino and polyvinyl alcohol silver halide emulsions onto a Web in distinct layer relationship comprising the steps of forming a coating bead of said liquid gelatino and said emulsions in bridging relation between the surface of the support and a stationary coating device spaced transversely therefrom, simultaneously feeding each of said liquid gelatino and said polyvinyl alcohol silver halide emulsions in the form of a layer into said head and in superposed relation with each other whereby the individual layers are maintained in distinct superposed relation, and continuously moving the surface of said support across and in contact with said head so that the surface of the support engages one of the outermost of the superposed. layers in said head and simultaneously picks up each of said layers and moves away from the bead with the liquid gelatino and polyvinyl alcohol silver halide emulsions in distinct superposed layers.
  • the method of simultaneously applying thin coatings of a plurality of like colloidal materials onto a web support in distinct layer relationship comprising the steps of making a solution of each of said colloidal materials, forming a coating bead of said solutions in bridging relation between the surface of the support and a coating device which is stationary relative to said bead and spaced transversely from said support, simultaneously feeding each of said solutions in the form of a layer into said bead and in superposed relation to the other solutions whereby the individual layers are maintained in distinct superposed relation, and producing a continuous relative movement between the bead and the surface of said support whereby the support moves across and in contact with said head and one surface of the support engages one of the outermost of the superposed layers in said bead and simultaneously picks up all of said layers and moves away from said head with the solutions in distinct superposed layers.
  • the method of simultaneously applying thin coatings of a plurality of difierent colloidal materials onto a web support in distinct layer relationship comprising the steps of making a solution of each of said colloidal materials, forming a coating bead of said solutions in bridging relation between the surface of the support and a coating device which is stationary relative to said head and spaced transversely from said support, simultaneously feeding each of said solutions in the form of a layer into said bead and in superposed relation .to the other solutions whereby the individual layers are maintained in distinct superposed relation, and producing a continuous relative movement between the bead and the surface of said support whereby the support moves across and in contact with said head and one surface of the support engages one of the outermost of the superposed layers in said bead and simultaneously picks up all of said layers and moves away from said bead with the solutions in distinct superposed layers.
  • the method of simultaneously applying thin coatings of a plurality of settable colloidal materials onto the surface of a flexible web support in distinct layer relationship comprising the steps of making a solution of each of said colloidal materials, forming a coating bead of said solutions in bridging relation between the surface of the support and a stationary coating device spaced transversely therefrom, simultaneously feeding each of said solutions in the form of a layer into said bead and in superposed relation to the other solutions whereby the individual layers are maintained in distinct superposed relation, continuously moving the surface of said 19 support across and in contact with said head so that the surface of the support engages one of the outermost of the superposed layers in said bead and simultaneously picks up all of said layers and moves away from the bead with the solutions in distinct superposed layers, and
  • vidual relative thicknesses depend upon the rate at which each solution is fed into the bead and whose combined thickness depends upon the speed of the support, setting said layers of deposited solutions to prevent flow thereof relative to the support, and then simultaneously drying the water from said deposited layers of solution.

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  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Textile Engineering (AREA)
  • General Physics & Mathematics (AREA)
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US489863A 1955-02-23 1955-02-23 Method of multiple coating Expired - Lifetime US2761791A (en)

Priority Applications (22)

Application Number Priority Date Filing Date Title
CA557259A CA557259A (en) 1955-02-23 Multiple layer hopper for multiply coating a web
CA557260A CA557260A (en) 1955-02-23 Multiple feed hopper for feeding a plurality of coating compositions
CA557258A CA557258A (en) 1955-02-23 Multilayer hopper for feeding a plurality of coating compositions
IT557307D IT557307A (ja) 1955-02-23
CA554506A CA554506A (en) 1955-02-23 Simultaneous deposition of a plurality of fluid coating materials
BE545464D BE545464A (ja) 1955-02-23
US489862A US2761418A (en) 1955-02-23 1955-02-23 Multiple coating apparatus
US489861A US2761417A (en) 1955-02-23 1955-02-23 Multiple coating apparatus
US489863A US2761791A (en) 1955-02-23 1955-02-23 Method of multiple coating
US489969A US2761419A (en) 1955-02-23 1955-02-23 Multiple coating apparatus
DEE11998A DE1211488B (de) 1955-02-23 1956-02-22 Vorrichtung zum gleichzeitigen Auftragen mehrerer Schichten
DEE11996A DE1208998B (de) 1955-02-23 1956-02-22 Vorrichtung zum gleichzeitigen Auftragen mehrerer Schichten
DEE11995A DE1151173B (de) 1955-02-23 1956-02-22 Verfahren zum Beschichten eines Schicht-traegers fuer einen photographischen Film
DEE11997A DE1216686B (de) 1955-02-23 1956-02-22 Vorrichtung zum gleichzeitigen Auftragen mehrerer Schichten
GB26305/59A GB834527A (en) 1955-02-23 1956-02-23 Improvements in or relating to web coating apparatus
GB5590/56A GB834525A (en) 1955-02-23 1956-02-23 Improved methods of making flexible material having a plurality of superposed layers
FR1148817D FR1148817A (fr) 1955-02-23 1956-02-23 Procédé et machine pour l'application simultanée de plusieurs couches sur un support et produit obtenu
GB26306/59A GB834528A (en) 1955-02-23 1956-02-23 Improvements in or relating to web coating apparatus
US769881A US2975754A (en) 1955-02-23 1958-10-27 Multiple coating apparatus
DEE18311A DE1177931B (de) 1955-02-23 1959-09-30 Vorrichtung zum gleichzeitigen Auftragen mehrerer Schichten
FR808185A FR1238160A (fr) 1955-02-23 1959-10-22 Machine pour l'application simlutanée de plusieurs couches sur un support en bande continue
GB36130/59A GB901686A (en) 1955-02-23 1959-10-26 Improvements in or relating to web coating apparatus

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
US489861A US2761417A (en) 1955-02-23 1955-02-23 Multiple coating apparatus
US489969A US2761419A (en) 1955-02-23 1955-02-23 Multiple coating apparatus
US489862A US2761418A (en) 1955-02-23 1955-02-23 Multiple coating apparatus
US489863A US2761791A (en) 1955-02-23 1955-02-23 Method of multiple coating
US769881A US2975754A (en) 1955-02-23 1958-10-27 Multiple coating apparatus

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US2761791A true US2761791A (en) 1956-09-04

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US489862A Expired - Lifetime US2761418A (en) 1955-02-23 1955-02-23 Multiple coating apparatus
US489863A Expired - Lifetime US2761791A (en) 1955-02-23 1955-02-23 Method of multiple coating
US489861A Expired - Lifetime US2761417A (en) 1955-02-23 1955-02-23 Multiple coating apparatus
US489969A Expired - Lifetime US2761419A (en) 1955-02-23 1955-02-23 Multiple coating apparatus
US769881A Expired - Lifetime US2975754A (en) 1955-02-23 1958-10-27 Multiple coating apparatus

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Application Number Title Priority Date Filing Date
US489862A Expired - Lifetime US2761418A (en) 1955-02-23 1955-02-23 Multiple coating apparatus

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Application Number Title Priority Date Filing Date
US489861A Expired - Lifetime US2761417A (en) 1955-02-23 1955-02-23 Multiple coating apparatus
US489969A Expired - Lifetime US2761419A (en) 1955-02-23 1955-02-23 Multiple coating apparatus
US769881A Expired - Lifetime US2975754A (en) 1955-02-23 1958-10-27 Multiple coating apparatus

Country Status (7)

Country Link
US (5) US2761418A (ja)
BE (1) BE545464A (ja)
CA (4) CA554506A (ja)
DE (5) DE1211488B (ja)
FR (2) FR1148817A (ja)
GB (4) GB834527A (ja)
IT (1) IT557307A (ja)

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CA557258A (en) 1958-05-13
US2761419A (en) 1956-09-04
DE1211488B (de) 1966-02-24
IT557307A (ja) 1900-01-01
US2761417A (en) 1956-09-04
GB834528A (en) 1960-05-11
DE1208998B (de) 1966-01-13
CA554506A (en) 1958-03-18
US2761418A (en) 1956-09-04
FR1238160A (fr) 1960-08-05
CA557260A (en) 1958-05-13
GB834525A (en) 1960-05-11
US2975754A (en) 1961-03-21
DE1216686B (de) 1966-05-12
BE545464A (ja) 1900-01-01
DE1177931B (de) 1964-09-10
FR1148817A (fr) 1957-12-16
GB901686A (en) 1962-07-25
DE1151173B (de) 1963-07-04
GB834527A (en) 1960-05-11
CA557259A (en) 1958-05-13

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