US3385699A - Process for processing electrophotosensitive layers - Google Patents

Process for processing electrophotosensitive layers Download PDF

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Publication number
US3385699A
US3385699A US383645A US38364564A US3385699A US 3385699 A US3385699 A US 3385699A US 383645 A US383645 A US 383645A US 38364564 A US38364564 A US 38364564A US 3385699 A US3385699 A US 3385699A
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United States
Prior art keywords
layer
electrophotosensitive
cured
resin
fatigue
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Expired - Lifetime
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US383645A
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English (en)
Inventor
Honjio Satoru
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Fujifilm Holdings Corp
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Fuji Photo Film Co Ltd
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    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G5/00—Recording members for original recording by exposure, e.g. to light, to heat, to electrons; Manufacture thereof; Selection of materials therefor
    • G03G5/02—Charge-receiving layers
    • G03G5/04—Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor
    • G03G5/05—Organic bonding materials; Methods for coating a substrate with a photoconductive layer; Inert supplements for use in photoconductive layers
    • G03G5/0528—Macromolecular bonding materials
    • G03G5/0592—Macromolecular compounds characterised by their structure or by their chemical properties, e.g. block polymers, reticulated polymers, molecular weight, acidity
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G11/00—Selection of substances for use as fixing agents
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G13/00—Electrographic processes using a charge pattern
    • G03G13/22—Processes involving a combination of more than one step according to groups G03G13/02 - G03G13/20
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G5/00—Recording members for original recording by exposure, e.g. to light, to heat, to electrons; Manufacture thereof; Selection of materials therefor
    • G03G5/02—Charge-receiving layers
    • G03G5/04—Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor
    • G03G5/05—Organic bonding materials; Methods for coating a substrate with a photoconductive layer; Inert supplements for use in photoconductive layers
    • G03G5/0503—Inert supplements
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G5/00—Recording members for original recording by exposure, e.g. to light, to heat, to electrons; Manufacture thereof; Selection of materials therefor
    • G03G5/02—Charge-receiving layers
    • G03G5/04—Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor
    • G03G5/08—Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor characterised by the photoconductive material being inorganic
    • G03G5/087—Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor characterised by the photoconductive material being inorganic and being incorporated in an organic bonding material

Definitions

  • This invention relates in general to a process for making visible electrostatic images and in particular to a process for processing electrophotosensitive layers for making visible electrostatic images.
  • the light fatigue (hereinafter is called simply fatigue) or the pre-exposure effect on the electrophotosensitive layer can be removed by placing the layer in a dark place for a long period of time, heating the layer in a dark place, or exposing the layer to corona discharge (e.g., to negative corona discharge in the case of using a zinc-oxide electrophotosensitive layer).
  • corona discharge e.g., to negative corona discharge in the case of using a zinc-oxide electrophotosensitive layer.
  • the degree of fatigue of an electrophotosensitive layer can be determined more exactly by observing the form of a charging time-surface potential curve than by measuring the charged potential on the layer. That is, an electrophotosensitive layer placed in a dark place for a long period of life shows a very steep rising slope in the charging time-surface potential curve whereas a light-exposed or fatigued electrophotosensitive layer shows an extremely gentle slope in the curve.
  • FIG. 1 is a graph showing the influence of pre-exposure on a rising curve by charging of an electrophotosensitive ice layfr using zinc oxide as the photoconductive material;
  • FIG. 2 is a graph showing recovering characteristics from fatigue of a cured electrophotosensitive layer and a non-cured electrophotosensitive layer.
  • an electrophotosensitive layer having a delayed recovering rate from fatigue viz., a pre exposed electrophotosensitive layer shows a gentle rising slope in the charging time-surface potential curve and no matter how long the charging procedure (corona discharging) is continued, the surface potential of the layer only approaches a saturated potential value, that is, does not exceed the saturated value, which is equal to or lower than about a half of a saturated potential value of the layer placed in a dark place.
  • An electrophotosensitive layer having a high recovering rate from fatique shows also a gentle rising slope in the charging time-surface potential curve when it is preexposed, but the gentleness of the slope is weak as compared with the above case and the saturated potential value is nearly that of the layer placed in a dark place.
  • thermosetting resin in a non-cured state has in general a very low polymerization degree and, therefore, the non-cured thermosetting resin causes many troubles when it is adopted as a binder for an electrophotosensitive layer through the use of such a resin is preferable in a point of recovering from fatigue.
  • thermosetting resin when used as a binder for an electrophotosensitive layer of office copying papers,
  • the coated film or layer is soft and retains an adhesive property
  • the copying paper is liable to adhere to other one or they cause so called locking when they are stored for a long period of time or in a comparatively high-temperature circumstance
  • the coated film or layer applied on the conductive material is soft, the film or layer is easily in- 3 jured mechanically, from where the conductive material is apt to rust and (5)
  • the layer containing the non-cured resin is softened adjacent to the gas heated portion by the heat of the gas flame, which makes the operation diflicult as well as spoils the working object.
  • an object of this invention is to provide a process for producing an electrophotosensitive layer having a lowered pre-exposure effect or a high recovering power from fatigue.
  • Another object of this invention is to provide a process for producing an electrophotosensitive layer having a lowered pre-exposure effect and improved mechanical strength by using a non-cured thermosetting resin as the binder.
  • Still another object of this invention is to provide a process for processing an electrophotosensitive layer containing a non-cured thermosetting resin as the binder to give the electrophotosensitive layer having a visible image and having an improved mechanical strength.
  • a further object of this invention is to provide improved electrophotosensitive materials suitable for various electrophotographic purposes, such as, ofiice copying papers, offset-printing masters, electrophotographic marking on conductive materials, and the like.
  • the inventor has found that a better result can be obtained in the case of using a non-cured setting or thermosetting resin as a binder for an electrophotosensitive layer by maintaining the resin in its non-cured state in the photosensitive layer during an electrophotographic treatment and adding, after an image is fomed on the layer, a curing accelerator, a curing catalyst, etc., to the layer (it is of course effective to heat the layer besides).
  • a curing agent may preferably be done in practice by dissolving or dispersing it in a solvent for fixing an image, but the treating agent may be added to the layer in an addditional step.
  • an alkyd resin which can be cured as is well known by the action of an organic peroxide and a salt of a heavy metal, such as, manganese and cobalt even at room temperature one of them may be contained preliminary in an electrophotosensitive layer and after the end of the electrophotographic treatment another may be added to the layer by spraying or impregnating, or both treating agents may be added after.
  • the invention has an advantage that the restriction of an electrophotosensitive layer to be conducted according to the process of this invention to light-exposure conditions prior to charging or pre-exposure conditions can be loosened as compared with the case where the electrophotosensitive layer contains as a binder the cured thermosetting resin.
  • the rust preventing power and weathering resistance of a conductive material applied with an electrophotosensitive layer having a desired image on it can be improved by the process of this invention. Furthermore, it frequently occurs in the case of cutting, after the electrophotographic marking on a conductor such as a steel plate, the steel plate by means of an automatic gas cutting machine placed on the steel plate that if the thermosetting resin is not cured the non-cured layer is softened by the heat of the gas flame and the wheels of the gas cutting machine slip on and injure the softened portion of the layer, which results in causing rust formation.
  • a practical cutting operation that those drawbacks are improved or completely removed by curing the layer in accordance with the process of this invention.
  • a hard film-forming material or a material which can be copolymerized or condensated with the binder in the layer may of course be added besides.
  • Example 1 Component: Parts 'by wt. Photoconductive zinc oxide powder Short-oil type alkyd resin varnish (soybean oilmodified; oil length 40%) (non-volatile matter 50%) 30 Low molecular weight silicone resin varnish (non-volatile matter 60%) 30 Toluene 20 Methyl ethyl ketone peroxide 0.5
  • the above composition was mixed for 20 hours in a porcelain ball mill.
  • Thus prepared homogeneous liquid was diluted with toluene and applied by spraying on a steel plate pre-coated with a wash primer in a coating thickness (after dried) of 2011..
  • the plate was allowed to evaporate oh the solvent for 20 hours at room temperature.
  • the layer was placed in darkness for 1 hour and exposed to a corona discharge, and the surface potential of the charged layer was determined to be about 400-450 volts by measuring.
  • the layer was subjected to an image exposure, a cascade development, and then fixing according to a conventional electrophotographic process.
  • As the fixing liquid the following mixture was used.
  • the developer and the electrophotosensitive layer were swelled or dissolved by the action of the fixing liquid whereby the image was fixed and simultaneously cobalt naphthenate was penetrated into the layer.
  • treated layer was placed for about 10 hours at room temperature, it became solvent-insoluble. This resulted from the alkyd resin and the silicon resin in the layer being cured by the co-operation of the methyl ethyl ketone peroxide contained in the layer and the cobalt naphthenate in the fixing liquid.
  • an electrophotosensitive layer was prepared by applying on a steel plate the above-mentioned coating liquid but added with 1 part by weight of cobalt naphthenate and after 24 hours the characteristics were measured, which was compared with the results obtained by measuring the characteristics of the layer prepared as mentioned above in the example prior to fixing, that is, the characteristics of the layer in the state before spraying the fixing liquid containing cobalt naphthenate.
  • the relative sensitivity is a reciprocal of a light-exposure quantity required for decreasing the surface potential to a half of the surface potentialprior to the light exposure.
  • FIG. 2 shows clearly the difference of the recovering power between non-cured and cured layers.
  • FIG. 2 two curves corresponding to non-cured and cured layers are shown about the recovering ratios of the initial surface potential to a period placed in a dark place after pre-exposed to 5,000 lux fluorescent lamp for 5 minutes, that is, the ordinate of FIG. 2 represents a relative value of the surface potential of the layers subjected to the preexposure, the surface potential (shown in the above table) after placed in a dark place being defined to be 100. From FIG. 2, it is concluded that it takes several hours to 10 hours for the cured layer to recover completely from fatigue, while the non-cured layer is recovered from fatigue practically in several minutes.
  • EXAMPLE 2 A shot-blast steel plate coated with the electrophotosensitive layer as in Example 1, which was cured after fixing and a shot-blast steel plate coated with the same layer in Example 1, which was maintained in the noncured state without the addition of the catalyst, were placed in an aqueous 3% NaCl solution for 100 hours. The swelled area and the rusted area of the non-cured layer were about /3 of those of the cured layer.
  • the portions closely adjacent to the cut lines were heated, which resulted in softening the portion of the non-cured layer, and the softened portion of the non-cured layer was injured when the portion was contacted with a torchsupporting means or with an operator, which caused a rust formation when the plate was exposed in air for a long period of time.
  • the cured layer was softened a little by heating and there were almost no such drawbacks as in the case of the noncured layer.
  • EXAMPLE 3 Component: Parts by wt. Photoconductive zinc-oxide powder Epoxy ester-modified alkyd resin varnish (nonvolatile matter 50%) Toluene 20 Methyl ethyl ketone peroxide 0.5
  • the coating liquid having the above composition was applied on a steel plate as in Example 1 to a dried thickness of 3035,u. After drying, the plate was placed for 20 hours in a dark place. While, the fixing solution same as in Example 1 was sprayed onto the above photosensitive layer and after dried at room temperature the plate was also placed for 20 hours in a dark place. It was observed in this case that workability for gas cutting of the layer was much improved as in Example 2 by the increase in the hardness of the layer.
  • Example 4 The composition as in Example 3 was applied on two art papers and after forming images on the layers electrophotographically one was fixed with a fixing liquid containing a catalyst, cobalt naphthenate and another was fixed with a fixing liquid without containing cobalt naphthenate.
  • thermosetting resin selected from the group consisting of alkyd resin and epoxy ester resin, which comprises maintaining said thermosetting resin in said layer in a non-cured state until the formation of a visible image on said layer by an electrophotognaphic process is finished, subjecting said layer to uniform charging, image exposure and development with dry developing powders, and after finishing the image formation, uniformly applying on the layer a solution of a curing agent selected from the group consisting of a curing catalyst, a curing accelerator and a material which can effect polymerization reaction or condensation reaction with the resin in the layer dissolved in a volatile organic solvent which can dissolve both the curing agent and the dry developing powders employed, whereby the thermosetting resin is cured and the developed image is permanently fixed.
  • a curing agent selected from the group consisting of a curing catalyst, a curing accelerator and a material which can effect polymerization reaction or condensation reaction with the resin in the layer dissolved in a volatile organic solvent which can dissolve both the curing agent and the dry developing powders employed, whereby the thermosetting resin is

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Photoreceptors In Electrophotography (AREA)
  • Fixing For Electrophotography (AREA)
US383645A 1963-07-25 1964-07-20 Process for processing electrophotosensitive layers Expired - Lifetime US3385699A (en)

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Application Number Priority Date Filing Date Title
JP3948963 1963-07-25

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US3385699A true US3385699A (en) 1968-05-28

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US383645A Expired - Lifetime US3385699A (en) 1963-07-25 1964-07-20 Process for processing electrophotosensitive layers

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US (1) US3385699A (en, 2012)
BE (1) BE651039A (en, 2012)
DE (1) DE1294198B (en, 2012)
DK (1) DK133069C (en, 2012)
GB (1) GB1072476A (en, 2012)
NL (2) NL6408500A (en, 2012)
SE (1) SE310458B (en, 2012)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3533783A (en) * 1967-07-31 1970-10-13 Eastman Kodak Co Light adapted photoconductive elements
US3961947A (en) * 1973-10-19 1976-06-08 Xerox Corporation Process for preparing waterless lithographic masters
USD306494S (en) 1987-10-07 1990-03-06 Bajusz Harold F Perfume applicator
US5888689A (en) * 1996-07-26 1999-03-30 Agfa-Gevaert, N.V. Method for producing cross-linked fixed toner images

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3192043A (en) * 1960-10-07 1965-06-29 Commw Of Australia Method for developing and fixing electrostatic images in initially partially cured base elements
US3226227A (en) * 1960-09-02 1965-12-28 Rca Corp Method of producing a solvent-resistant pattern using developed electrostatic image formation techniques
US3291738A (en) * 1960-09-02 1966-12-13 Rca Corp Materials for preparing etch resists

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1040900B (de) * 1956-08-28 1958-10-09 Agfa Ag Verfahren zur Herstellung von lichtleitfaehigen Schichten fuer elektrophotographische Verfahren

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3226227A (en) * 1960-09-02 1965-12-28 Rca Corp Method of producing a solvent-resistant pattern using developed electrostatic image formation techniques
US3291738A (en) * 1960-09-02 1966-12-13 Rca Corp Materials for preparing etch resists
US3192043A (en) * 1960-10-07 1965-06-29 Commw Of Australia Method for developing and fixing electrostatic images in initially partially cured base elements

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3533783A (en) * 1967-07-31 1970-10-13 Eastman Kodak Co Light adapted photoconductive elements
US3961947A (en) * 1973-10-19 1976-06-08 Xerox Corporation Process for preparing waterless lithographic masters
USD306494S (en) 1987-10-07 1990-03-06 Bajusz Harold F Perfume applicator
US5888689A (en) * 1996-07-26 1999-03-30 Agfa-Gevaert, N.V. Method for producing cross-linked fixed toner images

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NL6408500A (en, 2012) 1965-01-26
DK133069B (da) 1976-03-15
SE310458B (en, 2012) 1969-04-28
BE651039A (en, 2012) 1964-11-16
DE1294198B (de) 1969-04-30
GB1072476A (en) 1967-06-14
NL130806C (en, 2012)
DK133069C (da) 1976-08-09

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