US3671282A - Method of making an imaging member - Google Patents

Method of making an imaging member Download PDF

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Publication number
US3671282A
US3671282A US853869A US3671282DA US3671282A US 3671282 A US3671282 A US 3671282A US 853869 A US853869 A US 853869A US 3671282D A US3671282D A US 3671282DA US 3671282 A US3671282 A US 3671282A
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layer
substrate
plastic
softenable
particulate material
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US853869A
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William L Goffe
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Xerox Corp
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Xerox Corp
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    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G17/00—Electrographic processes using patterns other than charge patterns, e.g. an electric conductivity pattern; Processes involving a migration, e.g. photoelectrophoresis, photoelectrosolography; Processes involving a selective transfer, e.g. electrophoto-adhesive processes; Apparatus essentially involving a single such process
    • G03G17/10—Electrographic processes using patterns other than charge patterns, e.g. an electric conductivity pattern; Processes involving a migration, e.g. photoelectrophoresis, photoelectrosolography; Processes involving a selective transfer, e.g. electrophoto-adhesive processes; Apparatus essentially involving a single such process using migration imaging, e.g. photoelectrosolography

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  • This invention relates to imaging and in particular to a novel method of forming an imaging member.
  • a Xerographc plate containing a photoconductive insulating layer is first given a uniform electrostatic charge in order to sensitize its surface.
  • the plate is then exposed to an image of activating electromagnetic radiation such as light, X-ray or the like which selectively dissipates the charge in the illuminated areas of the photoconductive insulator, while leaving behind a latent electrostatic image in a non-lluminated area.
  • the latent electrostatic image may be developed and made visible by depositing finely divided electroscopic marking particles on the surface of the photoconductive insulating layer.
  • a Xerographic plate consists of a photoconductive layer comprising a substantially insulating organic resin binder having dispersed therein finely divided particles of an inorganic photoconductive insulating material.
  • This form of photoconductive plate is described in U.S. Patent 3,121,006 to Middleton et al., and other related patents in the field.
  • the binder plate shown by Middleton et al. can be formed by any convenient method such as those set forth in the disclosure of the above patent. These methods include forming a mixture of slurry of the materials which form the binder plate, and painting, pouring, dipping or spraying the material onto a suitable substrate to form the desired thickness of the photoconductive binder layer on the substrate.
  • the above methods involve forming a mixture of a slurry of the nert resinous binder material and the inorganic photoconductive insulating material, and other necessary ingredients, in order to form the binder plate.
  • the above methods result in a somewhat uneven control of the thickness of the photoconductive binder layer.
  • certain photoconductive particles may be dissolved, recrystallize, or chemically react adversely with particulate solvents and other chemical additives'in the slurry, and must be excluded from the above techniques necessary in manufacturing a binder plate.
  • imaging members are also used in a new migration imaging system embodiments of which are described in applicant's copending application Ser. No. 483,675 and described in applicant's copendng application Ser. No. 460,377, filed June 1, 1965 now U.S. Patent No. 3,520,- 681 which is a continuation-in-part of applicant's copending application Ser. No. 403,002, filed Oct. 12, 1964, now abandoned.
  • a limiting factor in the resolution of the images produced by an imaging process is the quality of the imaging member.
  • Binder layers may be made with the desired particles dispersed throughout the plastic matrix, or concentrated in one or more planar sections of the layer.
  • the substrate may or may not be allowed to harden prior to the subsequent coating of the surface. In most instances it will be desirable to allow the substrate to harden at least partially before another cycle of coating and softening of the substrate to aid in dispensing another coating of particles on the surface.
  • the occurrence of agglomeration or clustering of the particulate material is avoided or greatly reduced.
  • the particulate material does not agglomerate within the plastic substrate although the particulate material becomes very dense or concentrated in accordance with the process of this invention.
  • FIG. 1 is a schematic illustration of one method of making an imaging member contemplated by this invention.
  • FIG. 2 is a schematic illustration forming an imaging member.
  • FIG. 3 is a. schematic illustration of the second stage in forming an imaging member.
  • FIG. 4 is a schematic illustration of the third stage in forming an imaging member.
  • FIG. 5 is a view of one embodiment of a finished imagig member as contemplated by this invention
  • reference character denotes a conventional imaging member comprising an insulating substrate 11 having a conductive metallic overcoatng 12, and -a softenable plastic layer 13 overlaying layer 12.
  • the imaging member is formed preferably by cascading conventional carrier beads 14 having the desired particles to be coated 15, triboelectrically attracted to said carrier beads and being cascaded over the surface of the softenable plastic layer 13, whereby a sparse substantially uniform layer of the desired coating material 15 is formed on the surface of the softenable plastic layer 13, as shown in FIG. 2.
  • the coating applied to the plastic substrate is controlled so as to be, although substantially uniform, dispersed in relation to the area to be coated. That is, it has been found that agglomerates are avoided by applying to the plastic substrate a uniform but scatof the first stage of tered or dispersed layer of particulate material so as to the amount of particulate material on the carrier beads i and the amount of carrier beads being cascaded over the surface of the substrate, a dispersed or scattered uniform 'layer is easily provided.
  • a plurality of cascading Operations can be carried out between each embedment of the particles into the plastic substrate.
  • the plastic layer 13 is softened by any convenient means such as by Chemical vapors or liquids, or heat, so as to allow the deposited material 15 to snk into the softened plastic as shown in FIG. 3. Any softening means which only effects the plastic layer is suitable.
  • the cascading step illustrated in FIG. l is then carried out again forming another substantially uniform layer of particles 15 on layer 13 as shown in FIG. 4.
  • the softenable layer 13 is again softened as described in FIG. 3 so as to build up another layer of particles'in the softenable plastic matrix 13.
  • This process of cascading, softening, and then cascading again, is carried outany desired number of times until a sufficient thckness of cascadedparticles 15 are built up in the softenable plastic matrix layer 13.
  • This process results in a final plate such as that illustrated in FIG. 5 containing a coated substrate having thereon a layer comprising particles 15 dispersed in a plastic matrix 13.
  • the substrate upon which the softenable plastic is laid may be any conventional imaging type substrate such as a plastic film overcoated with a thin film of aluminum.
  • Any suitable xerographic substrate known to the art may be used. Typical substrates include a metallic sheet, a web, foil, cylinder, or the like; a sheet of glass with an electically conductive coating, or a conductive coated sheet of paper or stable plastic.
  • the conductive substrate in some instances may be deleted, if desired, and an insulating base used, or in some cases no substrate employed at all. If imaging systems other than Xerographic are used, the substrate may be either a conductor as defined above, semi-conductor or an insulator such as paper or plastic.
  • the softenable plastic material of layer 13 may be any suitable material which is heat, solvent vapor, or liquid softened. Suitable materials are Staybelite Ester 10, a difty percent hydrogenated glycerol rosin ester of the Hercules Powder Co., Piccotex 100, a styrene-type resin of Pennsylvania Industrial Chemical Co.; Araldite 6060 and 6071, epoxy resins of CIBA; Velsicol X-37, Velsicol Chemical Corporation. Other softenable materials useful in the practice of this invention are listed in copendng application Ser. No. 837,780 filed June 30, 1964 which is incorporated heren by reference. This group of plastic materials is not intended to be limiting, but merely illusrtative of materials suitable for the plastic matrix.
  • the plastic layer may be of any suitable thckness, electrically conductive or non-conductive.
  • the plastic substrate may be as thin as 1 to 4 microns in thckness, with no 'limitations on the maximum thckness.
  • Typical solvents include without limitation; cyclohexane, Freon 113, Sohio Odorless Solvent 3440, pentane, heptane, toluene, trichloroethylene, methyl ethyl ketone, methylene chloride, acetone, etc.
  • Exposure to the above solvents need only be as long as necessary to soften the plastic substrate. Times ranging from about a fewseconds or less up to about 30 seconds, depending upon the softening effect of the particular solvent, are usually sufficient. Vapor softening is preferred over softening by immersng in the liquid solvent in that liquid solvents may dissolve the substrate unless the exposure' is carefully controlled.
  • the temperature need only be as high as that necessary to allow the particulate material to embed into the plastic. Temperatures are usually in the range of about 60' to C. Times up to several minutes are usually suflicient.
  • the particles 15 which constitute the remaining portion of the binder layer may comprise any suitable photoconductive, conductive or insulating material.
  • Typical photoconductors are amorphous selenium, any of the inorganic photoconductive pigments disclosed in U.S. Pat. 3,121,006 to Middleton et al., which include zinc oxde, zinc sulfide, cadmium sulfide, cadmium sulfoselenide and many others, compounds of arsenic and selenium, organic photoconductors including azo dyes, such as Watchung Red B (E. I. du Pont de Nemours & Co.), quinacridones, such as Monastral Red B (E. I.
  • the particles 15 may be conductive or insulating depending on the structure desired. Any suitable insulating or conductve particles or pigments may be used. Typical materials are carbon black, garnet, iron oxide, pigment dyes such as prusson blue, and many other materials.
  • the carrier bead material 14 may comprise any suitable conventional carrier known to the art. Typical carrers are glass beads, plastic coated metal, coated glass, etc. The only requirement necessary in regard to the cascade material is that the proper triboelectric relationship between the carrier bead and "toner or particulate material be met. In general, the particle size of the carrier beads are up to about 700 microns in diameter.
  • the method of this invention results in the particles being dispersed in a layer to a depth of about M to of the thickness of the softenable plastic layer.
  • the size of the particulate material is normally small in comparison with the thickness of the plastic substrate, ranging in size up to about 30 microns in diameter. Usually, however, the particulate material ranges in size of about .01 to about 5 microns or less in diameter with much of the material being submicroscopic in size depending on the desired imaging member to be formed. For optimum image density, the particles size is below an average of about 0.7 micron. Obviously, there must be maintained some relationship between the size of the particulate material and the thickness of the softenable plastic substrate. That is, the size of the particle material must certainly not exceed the thickness of the substrate and desirably the diameter of the particles are not greater than about half the thickness of the softenable plastic layer.
  • the desired particulate material may be coated on the surface of the plastic substrate by dusting, spraying, vapor condensation, dipping in a fluidzed bed etc.
  • the coating step is repeated between each softening step and the amount of particulate material is maintained low so as to provide a dispersed coating on the surface of the substrate at any one time.
  • the plastic substrate may remain soft during the coating operation depending, of course, on the coating method selected.
  • the procedure for dyeing the zinc oxide comprises placing various amounts of zinc oxide and Rhodamine B dye in 25 ml. of methyl alcohol. The solution is then poured onto filter paper to dry. The resulting paste is stirred until all the alcohol has evaporated. The mixture is then baked for about 1 hour resulting in a dyed zinc oxide powder.
  • the carrier beads consist of glass beads 50 microns in diameter available from Potters Brothers, Inc.
  • the cascading mixture used in the examples consists of a .12 gram ratio of zinc oxide mixture (dyed with Rhodamine B) and 50 grams of glass beads.
  • Example I A strip of aluminized Mylar designated Sample 1, consisting of a micron layer of Myler overcoated with a submicron layer of aluminum, which has a 2 micron rollcoated overlayer of a softenable plastic. Staybelite 10 ⁇ thereon, is fixed to the bottom of a rectangular 2 x 6 x 4 nch brass container. The container is rotated about its horizontal axis and cascaded with a mixture of .12 gram of Florence Green Seal zinc oxide particles dyed with .03 gram of Rhodamine B per 8 grams of zinc oxide, and 50 grams of 50 micron diameter glass beads.
  • the developer material' consisting of carrier beads and zinc oxide particles, is cascaded over the aluminized Mylar strip held to the bottom of the container for 10 rotations of cascades.
  • the strip is removed from the container and heated to C. for two minutes, re-fixed in the container, and cascaded again. This cycle is repeated 6 times after which a zinc oxide binder layer has been formed With the zinc oxide particles dispersed approximately half way through the thickness of the softenable Staybelite plastic.
  • Example II Five additional strps designated Samples 2-6 are formed by the method of Example I using various mixtures as set forth in Table I and varying number of layers and cascades per layer. The mixtures, number of layers, and cascades per layer are illustrated in Table II below for Samples 1-6, inclusive.
  • Example III Example IV Sample 2 of Table II is treated by the imaging method of Example III by charging to an initial negative potential of 130 volts, and exposed to a light source .of 11.2 footcandle-seconds. r
  • Example V sample 3 of Table II is treated by the method of Example III by charging to an initial negative potential of 140 volts and exposed to a light source of 11.2foot-candleseconds.
  • Example VI Sample 4 of Table II is imaged by the method of Example III by charging to an initial negative potential of 150 volts and exposing to a light exposure of 84 foot-Candleseconds.
  • Example VII A strip of Staybelite coated 2 microns thick over a layer of aluminized Mylar is prepared as described in Example I. The strip is placed face up on a heated surface and heated to about 80 C. A powder cloud of charcoal containing 8.7X10- gms. of charcoal per liter of air is blown on to the surface of the softened Staybelite for a period of seconds whereupon the charcoal particles become attached to the Staybelite. After delay sufficient to allow the particles to become fully embedded below the surface, this procedure is repeated five times during which the substrate remains heated. The thus formed imaging member is imaged and developed in accordance with the procedure of Example VIII to produce a visible replica of the electrostatic image.
  • Example VIII An imaging member is made by first roll-coating a sheet of aluminized Mylar polyester film with a layer of Piccotex 100 approximately 2 microns in thickness. A mixture of air spun graphite particles (Type 200-19, The Joseph Dixon Crucible Co., Jersey City, NJ.) and 50 micron glass beads is then cascaded across the surface of the resin layer to form a sparse layer of the particles. The surface is heated to slightly above 100 C. whereupon the particles sink below the surface of the layer. Thisprocess is repeated until the graphite particles have been dispersed in the layer to a depth of approximately 1 micron.
  • An electrostatic image is applied to the member by means of a corona discharge devce and a stencil.
  • the image areas are positively charged to about 60 volts;
  • latent image-hearing member is then treated with cyclohexane vapor resulting in migration of the charged areas of particles to the surface of the polyester film'.
  • Nonimaged portions of particles and the layer of Piccotex are then removed by immersing the developed plate in liquid cyclohexane for about 10 seconds. The result is a faithful visible replica of electrostatic image.
  • Example IX-XI I 3 The procedure of Example VIII is carried out ⁇ with a series of imaging members to which are applied electrostatic images of 2, '20, '40 and 160 volts, respectively, instead of 60 volts as in Example VHI. Faithful visible replicas of the electrostatic image are produced. v i
  • nxam es XIILXXIX A series of seventeen imaging members is prepared by cascading a mixture of graphite particles (as used in Example VIII) and 750 micron glass .beads several times across the surface of a two micron layer of Staybelite 10 (Hercules Powder Company) overlying aluminized Mylar polyester film. The particles are embedded below the surface of the layer as in Example I. An electrostatic image is then formed on each member by means of a corona discharge device and mask, and the members are developed immersion in liquid solverts'. to form faithful replicas, in accordance with .the following:
  • a Thevinstant imaging process can also be cared out with the materials and values shown below in Table IV.
  • the substrate comprses aluminized Mylar over which a layer of softenable material is roll coated.
  • the particles in a plastic substrate is formed by the cascade method described above. Development is by immersion in solvent liquid.
  • the garnet particles used has an average diameter of about 5 microns.
  • Freon 113 Cyclohexane. Freon 113. 7- Cyclohexane.
  • step (c) repeating steps (a) and (b) a plurality of times whereby previously embedded particulate material further disperses in said substrate to provide a substantally unagglomerated visible dsperso of said material in said substrate.
  • step (a) is repeated a plurality of times to build up the layer of particulate material to be embedded in said substrate to no more than a monolayer.
  • step (e) repeating steps (b), (c) and (d) at least once 'whereby previously embedded particulate material further disperses in said substrate to provide a substantially uragglomerated visible dispersion of said material in said substrate.
  • step (b) is repeated a plurality of times prior to each repeat of steps (c) and (d) to build up the layer of particulate material to be embedded in said substrate to no more than a monolayer.
  • a method of forming an maging member comprising:
  • step (e) repeating steps (b), (c) and (d) at least once whereby previously embedded particulate material further disperses in said substrate to provide a substantially unagglomerated visible dispersion of said material in said substrate.
  • a method of making an maging member comprising:
  • step (e) repeating steps (b), (c) and (d) at least once whereby previously embedded particulate material further disperses in said substrate to provide a substantially unagglomerated visible dispersion of said material in said substrate.
  • step (b) is accomplished a plurality of times prior to each repeat of steps (c) and (d) to build up the layer of particulate material to no more than a monolayer.
  • the photoconductive material comprises amorphous selenium.
  • steps '(b) and (c) are accomplshed a sufficient number of times so that particles are dispersed in said softenable substrate layer to between about fl to about of the thickness of said layer.

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  • Photoreceptors In Electrophotography (AREA)
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US853869A 1969-08-28 1969-08-28 Method of making an imaging member Expired - Lifetime US3671282A (en)

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BE (1) BE755384A (fr)
DE (1) DE2042846A1 (fr)
FR (1) FR2059927A5 (fr)
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4757472A (en) * 1986-12-31 1988-07-12 Tecon Memory, Inc. Electrophotographic optical memory system
US4875520A (en) * 1985-10-22 1989-10-24 Airxchange, Inc. Desiccant heat device
US6048572A (en) * 1996-09-26 2000-04-11 National Label Company Method and apparatus for making thermochromic battery tester

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2270574B (en) * 1992-09-15 1996-05-01 Xerox Corp Method of making electrophotographic and ionographic imaging members

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4875520A (en) * 1985-10-22 1989-10-24 Airxchange, Inc. Desiccant heat device
US4757472A (en) * 1986-12-31 1988-07-12 Tecon Memory, Inc. Electrophotographic optical memory system
US6048572A (en) * 1996-09-26 2000-04-11 National Label Company Method and apparatus for making thermochromic battery tester

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GB1326056A (en) 1973-08-08
FR2059927A5 (fr) 1971-06-04
NL7012614A (fr) 1971-03-02
DE2042846A1 (de) 1971-03-11
BE755384A (fr) 1971-03-01

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