Classifications

• • 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
• • 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
  • G03G5/0525—Coating methods
• • 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
  • G03G5/0557—Macromolecular bonding materials obtained otherwise than by reactions only involving carbon-to-carbon unsatured bonds
  • G03G5/0564—Polycarbonates
• • 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
  • G03G5/14—Inert intermediate or cover layers for charge-receiving layers
  • G03G5/147—Cover layers
  • G03G5/14708—Cover layers comprising organic material
• • 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
  • G03G5/14—Inert intermediate or cover layers for charge-receiving layers
  • G03G5/147—Cover layers
  • G03G5/14708—Cover layers comprising organic material
  • G03G5/14713—Macromolecular material
  • G03G5/14747—Macromolecular material obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
  • G03G5/14756—Polycarbonates
• • H—ELECTRICITY
  • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
  • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
  • H05B33/00—Electroluminescent light sources
  • H05B33/10—Apparatus or processes specially adapted to the manufacture of electroluminescent light sources

Definitions

• he present invention relates to a method of producing an electrophotographic photosensitive member, a method of producing an organic device, and an emulsion for a charge transporting layer.
• electrophotosensitive member containing an organic photocondu ' ctive substance
• the organic electrophotographic photosensitive member has been a mainstream electrophotographic
• electrophotographic photosensitive members a laminated electrophotographic photosensitive member has been frequently used.
• the laminated electrophotographic photosensitive member improves its features by
• a method involving dissolving a functional material in an organic solvent to produce an application solution and applying the solution onto a support has been generally employed as a method of producing the laminated electrophotographic photosensitive member.
• a charge transporting layer is often required to have durability. Accordingly, the thickness of a coat of the application liquid for the charge transporting layer is larger than that of any other layer and hence the usage of the application liquid for the charge transporting layer is also large. As a result, the layer uses a large amount of the organic solvent. To curtail the usage of the organic solvent at the time of the production of the electrophotographic photosensitive member, the amount of the organic solvent to be used in the application liquid for the charge transporting layer is desirably curtailed. However, the production of the application liquid for the charge transporting layer requires the use of a halogen-based solvent or an aromatic organic solvent because a charge transporting substance and a resin each have high solubility in any such solvent.
• Patent Literature 1 reports an effort to curtail the
• This literature discloses that an emulsion for the charge transporting layer is produced by forming oil droplets of an organic solution, which is prepared by dissolving a substance to be incorporated into the charge transporting layer in an organic solvent, in water .
• electrophotographic photosensitive member by which, in a method of forming a charge transporting layer, the stability of an application liquid for a charge
• the present invention is also directed to providing a method of producing an organic device.
• the present invention is directed to
• he present invention provides a method of producing an electrophotographic photosensitive member which
• the method including the steps of:
• preparing a solution including:
• he present invention also provides a method of
• the present invention also provides an emulsion for a charge transporting layer, including a solution
• the solution includes: a first liquid whose solubility in water under 25°C and 1 atmosphere is 1.0 massl or less; a second liquid whose solubility in water under 25°C and 1 atmosphere is 5.0 massl or more; a charge transporting substance; and a binder resin.
• the stability of the emulsion after its long-term storage is improved and the charge transporting layer having high uniformity is formed.
• the emulsion for a charge transporting layer having high stability after its long-term storage is improved.
• FIGURE is a view illustrating an example of the
• apparatus including a process cartridge having an electrophotographic photosensitive member of the
• photosensitive member of the present invention includes the steps of: preparing a solution containing a first liquid whose solubility in water under 25°C and 1 atmosphere is 1.0 mass% or less, a second liquid whose solubility in water under 25°C and 1 atmosphere is 5.0 mass% or more, a charge transporting substance, and a binder resin, followed by the dispersion of the
• the second liquid be at least one kind selected from the group consisting of
• invention is a substance having hole transporting performance, and examples thereof include a
• butadiene compound and an enamine compound.
• a triarylamine compound is preferably used as the charge transporting substance in terms of improvements in electrophotographic characteristics.
• binder resin constituting the charge transporting layer examples include a styrene resin, an acrylic resin, a polycarbonate resin, and a polyester resin. Of those, a polycarbonate resin or a polyester resin is preferred. A polycarbonate resin having a repeating structural unit represented by the following formula (2) or a polyester resin having a repeating structural unit represented by the following formula (3) is more preferred.
• X 1 represents a single bond, a methylene group, an
• X 2 represents a single bond, a methylene group, an ethylidene group, a propylidene group, a
• Y represents an m-phenylene group, a p-phenylene group, or a divalent group having two p-phenylene groups bonded via an oxygen atom.
• the weight-average molecular weight of the binder resin is a weight-average
• an additive may be incorporated into the charge transporting layer.
• the additive constituting the charge transporting layer include an antidegradant such as. an antioxidant, a UV absorber, or a light stabilizer, and releasability- providing resins.
• the antidegradant include a hindered phenol-based antioxidant, a hindered amine-based light stabilizer, a sulfur atom-containing antioxidant, and a phosphorus atom-containing
• releasability-providing resins include a fluorine atom-containing resin and a resin containing a siloxane structure.
• the charge transporting substance and the binder resin are each soluble in the first liquid or the second liquid.
• the first liquid is a hydrophobic liquid whose solubility in water under 25 °C and 1 atmosphere is 1.0 mass% or less
• the second liquid is a hydrophilic liquid whose solubility in water under 25°C and 1 atmosphere is 5.0 mass% or more.
• the second liquid is more preferably a hydrophilic liquid whose solubility in water under 25°C and 1 atmosphere is 20.0 mass% or more.
• Table 1 shows representative examples of the hydrophobic liquid as the first liquid and Table 2 shows representative examples of the hydrophilic liquid as the second liquid, but the first liquid and the second liquid in the present invention are not limited thereto.
• aqueous solubility in each of Tables 1 and 2 refers to a solubility in water under 25°C and 1 atmosphere (atmospheric pressure) represented in a mass% unit.
• Two or more kinds of the first liquids as hydrophobic liquids may be used as a mixture.
• hydrophilic liquids each serving as the second liquid ether-based solvents are preferred.
• solvents at least one of tetrahydrofuran and dimethoxymethane is more preferred from the viewpoint of the stability of the emulsion.
• wo or more kinds of the second liquids as hydrophilic liquids may be used as a mixture.
• a hydrophilic liquid having a relatively low boiling point specifically, a boiling point of 100°C or less is more preferably used from the viewpoint of film uniformity because a
• dispersion medium is quickly removed in the step of forming a film by heating.
• a ratio (a/b) of the mass of the first liquid (a) to the mass of the second liquid (b) is preferably 1/9 to 9/1.
• the percentage of the second liquid is more preferably the higher because, in the step of preparing the emulsion to be described later, an oil droplet is reduced in diameter when emulsified and hence the emulsion is additionally stable.
• transporting substance and the binder resin in the solution of the first liquid and the second liquid preferably falls within such a range that the charge transporting substance and the binder resin dissolve to provide a solution, and that the solution has a proper viscosity at the time of emulsion from the viewpoint of the preparation of a stable emulsion. More
• the charge transporting substance and the binder resin are preferably dissolved at a ratio in the range of 10 mass or more and 50 mass3 ⁇ 4 or less in the solution of the first liquid and the second liquid.
• the viscosity of the solution in which the charge transporting substance and the binder resin have been dissolved preferably falls within the range of 50 mPa ⁇ s or more and 500 mPa ⁇ s or less.
• An existing emulsification method may be employed as an emulsification method of preparing the emulsion.
• the emulsion contains at least the charge transporting substance and the binder resin in a state where the substance and the resin are at least
• a stirring method and a high-pressure impact method are described below as specific emulsification methods, but the production method of the present invention is not limited thereto.
• the water to be used as the dispersion medium is preferably ion-exchanged water obtained by removing a metal ion and the like with an ion exchange resin or the like from the viewpoints of electrophotographic characteristics.
• the conductivity of the ion-exchanged water is preferably 5 yS/cm or less.
• the stirring machine is preferably a stirring machine capable of high-speed stirring because the solution can be
• stirring machine examples include a homogenizer
• the emulsion can be prepared by: dissolving the charge transporting substance and the binder resin in the first liquid and the second liquid to prepare a solution; weighing the solution; weighing water as a dispersion medium; mixing the solution and the water; and causing the contents of the mixed liquid to impact with each other under high pressure.
• the emulsion may be prepared by causing the solution and the water as different liquids to impact with each other without mixing the liquids.
• apparatus to be used in the method is, for example, a "Microfluidizer M-110EH” manufactured by Microfluidics in the U.S., or a “Nanomizer YSNM-2000AR” manufactured by YOSHIDA KIKAI CO., LTD.
• the transporting substance (ct) , the mass of the binder resin (r) , the mass of the first liquid (a) , and the mass of the second liquid (b) in the emulsion is preferably 3/7 to 8/2, more preferably 5/5 to 7/3 from the viewpoint of the stability of the emulsion.
• the percentage of the water is preferably the higher from such a viewpoint that an oil droplet is reduced in diameter when emulsified and the emulsion is stable. Accordingly, the ratio can be adjusted so that an oil droplet may be reduced in diameter and the stability of the emulsion may be additionally improved to such an extent that the charge transporting substance and the binder resin dissolve in the organic solvents.
• the ratio of the charge transporting substance and the binder resin in an oil droplet is preferably 10 to 50 massl with respect to the organic solvents.
• a ratio between the charge transporting substance and the binder resin falls within the range of preferably 4:10 to 20:10 (mass ratio), more preferably 5:10 to 12:10 (mass ratio) .
• the additive when the additive is further added to the charge transporting substance and the binder resin, its content is preferably 50 mass% or less, more preferably 30 mass% or less with respect to the solid content ratio of the charge
• a surfactant may be incorporated into the emulsion of the present invention for the purpose of additionally stabilizing its emulsification .
• the surfactant is preferably a nonionic surfactant from the viewpoint of suppressing the deterioration of the electrophotographic characteristics.
• the nonionic surfactant is, for example, a surfactant whose
• hydrophilic portion is a nonelectrolyte , in other words, a surfactant having a hydrophilic portion that does not ionize, and specific examples thereof include a series of nonionic surfactants out of: a NOIGEN series
• ADEKA NOL series manufactured by ADEKA CORPORATION; and a NEWCOL series manufactured by NIPPON NYUKAZAI CO., LTD.
• One kind of those surfactants may be used alone, or two or more kinds thereof may be used in combination.
• a surfactant having a hydrophilic- lipophilic balance (HLB) in the range of 8 to 15 is preferably selected for the stability of the emulsion.
• the addition amount of the surfactant is preferably as small as possible from such a viewpoint that the
• the surfactant may be added to the water as a dispersion medium in advance, or may be added to the organic solvents in which the charge transporting substance and the binder resin have been dissolved. Alternatively, the surfactant may be added to each of both the water and the organic solvents before the emulsification .
• the incorporation of not a hydrophobic organic solvent alone but both hydrophobic and hydrophilic organic solvents has significantly improved the stability of the emulsion as compared with that in the case where an emulsion is produced with the hydrophobic organic solvent alone. The reason for the foregoing is described later.
• the surfactant may be added to the water as a dispersion medium in advance, or may be added to the organic solvents in which the charge transporting substance and the binder resin have been dissolved. Alternatively, the surfactant may be added to each of both the water and the organic solvents before the emulsification .
• emulsion for a charge transporting layer may contain an additive such as a defoaming agent or a viscoelasticity modifier to such an extent that an effect of the present invention is not impaired.
• particles prepared as described above preferably falls within the range of 0.1 to 20.0 ⁇ , and more preferably falls within the range of 0.1 to 5.0 ym from the viewpoint of the stability of the emulsion.
• any one of the existing application methods such as a dip coating method, a ring coating method, a spray coating method, a spinner coating method, a roller coating method, a Meyer bar coating method, and a blade coating method is adaptable.
• dip coating is a technique that is a technique that is a technique that is a technique that is a technique that is a technique that is a technique that is a technique that is a technique that is a technique that has a dip coating method, a ring coating method, a spray coating method, a spinner coating method, a roller coating method, a Meyer bar coating method, and a blade coating method.
• dip coating is a dip coating method, a ring coating method, a spray coating method, a spinner coating method, a roller coating method, a Meyer bar coating method, and a blade coating method.
• the emulsion of the present invention can be applied onto the support by the step.
• the charge transporting layer is formed on the support by heating the coat formed by the step of forming the coat.
• the emulsion is formed into a film in an additionally uniform fashion by bringing emulsified particles into close contact with each other simultaneously with the removal of the dispersion medium by the heating step. Accordingly, the particle diameters of the emulsified particles are preferably reduced in an additional fashion because a thickness distribution having high uniformity is obtained quickly after the removal of the dispersion medium.
• the temperature for the heating is preferably 100°C or more. Further, the heating temperature is preferably equal to or higher than the melting point of a charge
• the charge transporting substance is melted by the heating at a temperature equal to or higher than the melting point of the charge transporting substance, and then the binder resin dissolves in the melt of the charge transporting substance. As a result, a coat having high uniformity can be formed.
• the heating temperature is preferably performed at a temperature higher than the melting point of the charge transporting substance having the lowest melting point out of the charge transporting substances constituting the charge transporting layer by 5°C or more.
• the heating temperature is preferably 200°C or less because an excessively high heating temperature causes the denaturation or the like of the charge transporting substance .
• the thickness of the charge transporting layer produced by the production method of the present invention is preferably 3 ⁇ or more and 50 ⁇ or less, more
• the solution containing the charge transporting substance and the binder resin is prepared with the organic solvents containing both the hydrophobic and hydrophilic solvents, and then the emulsion is prepared by dispersing the solution in water. Accordingly, even when the emulsion is stored for a long time period, the agglomeration of the emulsion is suppressed, which is a result advantageous in terms of productivity.
• the production method of preparing the emulsion including dissolving the charge transporting substance and the binder resin with the organic solvents containing both the hydrophobic and hydrophilic solvents, and then dispersing the solution in water to prepare the
• the hydrophilic organic solvent in an oil droplet quickly migrates toward an aqueous phase side and hence the oil droplet becomes additionally small, and the concentration of each of the charge
• an emulsified particle adopts a form close to a fine particle of a solid and hence the occurrence of the agglomeration of oil droplets can be significantly suppressed as. compared with that in the case where an emulsion is prepared with the hydrophobic solvent alone. It is also
• the hydrophilic organic solvent in the organic solvents has such amphipathic property as to dissolve in both water and oil, and hence the solvent serves like a surfactant in an oil droplet particle to suppress the agglomeration (coalescence) of the oil droplets.
• the dispersed state can be maintained even after the long-term storage of the emulsion .
• photosensitive member produced by the method of producing an electrophotographic photosensitive member of the present invention is described.
• electrophotographic photosensitive member of the present invention is a method of producing an
• electrophotographic photosensitive member having a support, and a charge generating layer and a charge transporting layer on the support.
• photosensitive layer on a cylindrical support is widely used, but the member may be formed into a belt or sheet shape .
• he support has preferably electro-conductivity
• conductive support and a support made of a metal or an alloy such as aluminum, an aluminum alloy, or
• the support to be used may be an ED tube or an EI tube or one obtained by subjecting the tube to cutting, electrochemical buffing, or a wet- or dry-honing process.
• a support made of a metal or a support made of a resin having layer obtained by forming aluminum, an aluminum alloy, or an indium oxide-tin oxide alloy into a film by means of vacuum deposition may be used.
• a support obtained by impregnating conductive particles such as carbon black, tin oxide particles, titanium oxide particles, or silver particles in a resin or the like, or a plastic having an conductive resin may be used.
• the surface of the support may be subjected to, for
• cutting treatment for example, cutting treatment, roughening treatment, or alumite treatment.
• An conductive layer may be provided between the support and an intermediate layer or a charge generating layer to be described later.
• the conductive layer is formed through the use of an application liquid for the
• conductive layer which is prepared by dispersing conductive particles in a resin.
• the conductive particles include carbon black, acetylene black, metal or alloy powders made of, for example, aluminum, nickel, iron, nichrome, copper, zinc, and silver, and metal oxide powders made of, for example, conductive tin oxide and ITO.
• examples of the resin include a polyester resin, a polycarbonate resin, a polyvinyl butyral resin, an acrylic resin, a silicone resin, an epoxy resin, a melamine resin, a urethane resin, a phenol resin, and an alkyd resin.
• a solvent to be used for the application liquid for the conductive layer there are given, for example, an ether-based solvent, an alcohol-based solvent, a ketone-based solvent, and an aromatic hydrocarbon solvent .
• he thickness of the conductive layer is preferably 0.2 ⁇ or more and 40 ⁇ or less, more preferably 1 ⁇ or more and 35 m or less, still more preferably 5 ⁇ or more and 30 ⁇ or less.
• the intermediate layer may be provided between the
• the intermediate layer can be formed by applying an
• Examples of the resin in the intermediate layer include polyacrylic acids, methylcellulose, ethylcellulose, a polyamide resin, a polyimide resin, a polyamideimide resin, a polyamide acid resin, a melamine resin, an epoxy resin, a polyurethane resin, and a polyolefin resin.
• the resin in the intermediate layer is
• thermoplastic resin preferably a thermoplastic resin, and specifically, a thermoplastic polyamide resin or a polyolefin resin is preferred.
• the polyamide resin is preferably copolymer nylon with low crystallinity or no crystallinity which can be applied in a solution state.
• the polyolefin resin is preferably in a state where the resin can be used as a particle dispersion. It is more preferred that the polyolefin resin be dispersed in an aqueous medium.
• he thickness of the intermediate layer is preferably .0.05 ⁇ or more and 7 ⁇ or less, more preferably 0.1 ⁇ or more and 2 ⁇ or less.
• the intermediate layer may further contain
• the charge generating layer is provided on the support, conductive layer, or intermediate layer.
• Examples of the charge generating substance to be used in the electrophotographic photosensitive member of the present invention include azo pigments, phthalocyanine pigments, indigo pigments, and perylene pigments. Only one kind of those charge generating substances may be used, or two or more kinds thereof may be used. Of those, metallophthalocyanines such as oxytitanium phthalocyanine, hydroxygallium phthalocyanine, and chlorogallium phthalocyanine are particularly preferred because of their high sensitivity.
• binder resin to be used in the charge generating layer examples include a polycarbonate resin, a polyester resin, a butyral resin, a polyvinyl acetal resin, an acrylic resin, a vinyl acetate resin, and a urea resin.
• a butyral resin is particularly preferred.
• One kind of those resins may be used alone, or two or more kinds thereof may be used as a mixture or as a copolymer.
• the charge generating layer can be formed by applying an application liquid for the charge generating layer, which is prepared by dispersing a charge generating substance together with a resin and a solvent, and then drying the application liquid. Further, the charge generating layer may also be a deposited film of a charge generating substance.
• Examples of the dispersion method include one using a homogenizer, an ultrasonic wave, a ball mill, a sand mill, an attritor, or a roll mill.
• a ratio between the charge generating substance and the resin falls within the range of preferably 1:10 to 10:1 (mass ratio), particularly preferably 1:1 to 3:1 (mass ratio) .
• the solvent to be used for the application liquid for the charge generating layer is selected depending on the solubility and dispersion stability of each of the resin and charge generating substance to be used.
• the solvent examples include organic solvents such as an alcohol-based solvent, a sulfoxide-based solvent, a ketone-based solvent, an ether-based solvent, an ester-based solvent, and an aromatic hydrocarbon- solvent.
• organic solvents such as an alcohol-based solvent, a sulfoxide-based solvent, a ketone-based solvent, an ether-based solvent, an ester-based solvent, and an aromatic hydrocarbon- solvent.
• any of various sensitizers, antioxidants, UV absorbers, plasticizers , and the like may be added to the charge generating layer, if required.
• An electron transporting substance or an electron accepting substance may be added to the charge generating layer, if required.
• substance may also be incorporated into the charge generating layer to prevent the flow of charge from being disrupted in the charge generating layer.
• the charge transporting layer is provided on the charge generating layer.
• the charge transporting layer is produced by the
• a variety of additives may be added to each layer of the electrophotographic photosensitive member.
• additives examples include: an antidegradant such as an antioxidant, a UV absorber, or a light stabilizer; and fine particles such as organic fine particles or inorganic fine particles.
• an antidegradant such as an antioxidant, a UV absorber, or a light stabilizer
• fine particles such as organic fine particles or inorganic fine particles.
• the antidegradant include a hindered phenol-based antioxidant
• organic fine particles include polymer resin particles such as fluorine atom-containing resin particles, polystyrene fine particles, and polyethylene resin particles.
• examples of the inorganic fine particles include metal oxides such as silica and alumina.
• any of the application methods may be employed, such as a dip coating method, a spraying coating method, a spinner coating method, a roller coating method, a Meyer bar coating method, and a blade coating method.
• the forming method include: a method involving spraying the surface with abrasive particles to form the hollow-shaped unevenness; a method involving bringing a mold having the a hill-and- dale shape into press contact with the surface to form the hollow- and hill-shaped unevenness; and a method involving irradiating the surface with laser light to form the hollow-shaped unevenness.
• the method involving bringing the mold having the hill-and- dale shape into press contact with the surface of the surface layer of the electrophotographic photosensitive member to form the hollow- and hill-shaped unevenness is preferred.
• FIGURE illustrates an example of the schematic
• FIGURE a cylindrical electrophotographic image
• photosensitive member 1 is rotationally driven about an axis 2 in a direction indicated by an arrow at a predetermined peripheral speed.
• the surface of the electrophotographic photosensitive member 1 to be rotationally driven is uniformly charged to a positive or negative predetermined potential by charging unit (primary charging unit: a charging roller or the like) 3.
• charging unit primary charging unit: a charging roller or the like
• the surface receives exposure light (image exposure light) 4 output from exposing unit (not shown) such as slit exposure or laser beam scanning exposure.
• electrophotographic photosensitive member 1 are provided.
• transfer material P sequentially transferred onto a transfer material (such as paper) P by a transfer bias from transferring unit (such as a transfer roller) 6. It should be noted that the transfer material P is taken out. of transfer material-supplying unit (not shown) and fed into a gap between the electrophotographic photosensitive member 1 and the transferring unit 6 (abutting portion) in synchronization with the rotation of the
• the transfer material P onto which the toner images have been transferred is separated from the surface of the electrophotographic photosensitive member 1 and then introduced to fixing unit 8. The transfer
• material P is subjected to image fixation to be printed out as an image-formed product (print or copy) to the outside of the apparatus.
• electrophotographic photosensitive member 1 is
• pre-exposure light (not shown) from pre-exposing unit (not shown) and then repeatedly used in image formation.
• pre-exposure light not shown
• the charging unit 3, the developing unit 5, the transferring unit 6, and the cleaning unit 7, a plurality of them may be stored in a container and integrally supported to form a process cartridge.
• the process cartridge may be designed so as . to be detachably mountable to the main body of an electrophotographic apparatus such as a copying machine or a laser beam printer.
• the charging unit 3, the developing unit 5, and the cleaning unit 7 are integrally supported with the electrophotographic photosensitive member 1 to provide a cartridge, and then the cartridge is used as a process cartridge 9 detachably mountable to the main body of the electrophotographic apparatus with a guiding unit 10 such as a rail of the main body of the electrophotographic apparatus.
• An emulsion containing a charge transporting substance and a resin was produced by the following method.
• the emulsion was visually observed and then evaluated for the particle diameters of its emulsified particles. Further, the prepared emulsion was left to stand still for 2 weeks (under an environment having a temperature of 23°C and a humidity of 50%).
• the emulsion that had been left to stand still was stirred with a homogenizer PHYSCOTRON manufactured by MICROTEC CO., LTD. at 1,000 revolutions/min for 3 minutes. The state of the emulsion after the stirring was visually observed.
• the particle diameters of the emulsified particles were measured by measuring their average particle diameters before the standing and after the stirring with the homogenizer after the standing. It should be noted that, with regard to the measurement of the average particle diameters, the emulsion for a charge transporting layer was diluted with water and then the average particle diameter of the diluted liquid was measured with an
• Emulsions were each produced by the same method as that of Example 1 except that: the kinds and ratios of the charge transporting substances and the binder resin were changed as shown in Table 3; and the ratio of the hydrophobic organic solvent to the hydrophilic organic solvent and the kinds of the organic solvents, and the ratio of water to the organic solvents were changed as shown in Table 4.
• Table 4 shows the results of the evaluation of the resultant emulsions for their liquid stability .
• Table 4 shows the results of the evaluation of the resultant emulsions for their liquid stability.
• Table 4 shows the results of the evaluation of the resultant emulsions for their liquid stability.
• Table 4 shows the results of the evaluation of the resultant emulsions for their liquid stability.
• Emulsions were each produced by the same method as that of Example 1 except that: the kinds and ratios of the charge transporting substances and the binder resin were changed as shown in Table 3; the ratio of the hydrophobic organic solvent to the hydrophilic organic solvent and the kinds of the organic solvents, and the ratio of water to the organic solvents were changed as shown in Table 4; and a surfactant was added in an amount shown in Table 4 to water.
• Table 4 shows the results of the evaluation of the resultant emulsions for their liquid stability.
• the addition amount of the surfactant is represented as a ratio with respect to the entirety of an emulsion in a mass% unit.
• An application liquid containing a charge transporting substance and a binder resin was produced by the following method based on the method described in
• Patent Literature 1 1
• the emulsion for a charge transporting layer produced by the foregoing method was left to stand still for 2 weeks (under an environment having a temperature of 23 °C and a humidity of 50%).
• the emulsion for a charge transporting layer that had been left to stand still was stirred with a homogenizer at 1,000 revolutions/min for 3 minutes.
• the state of the dispersion (emulsion) after the stirring with the homogenizer was visually observed. The average
• Comparative Example 8 The resultant emulsion for a charge transporting layer was evaluated for its stability by the same method as that of Comparative Example 1. Table 6 shows the results.
• Example 56 (1-1) (1-5) 7/3 (2-1) 10/10
• Example 57 (1-1) (1-5) 7/3 (2-1) 10/10
• Example 202 (1-1) (1-5) 8/2 (2-1) 10/10
• Example 206 (1-1) (1-5) 8/2 (2-1) 10/10
• the method is not preferred because the surfactant is generally liable to cause the deterioration of the characteristics of an electrophotographic photosensitive member.
• the second liquid as a hydrophilic liquid in an oil droplet quickly migrates toward an aqueous phase side and hence the oil droplet becomes additionally small
• an emulsified particle adopts a form close to a fine particle of a solid and hence the occurrence of the agglomeration of oil droplets can be significantly
• the emulsion is useful as an application liquid for an
• the application liquid for the conductive layer was applied onto the aluminum cylinder by dip coating and hardened (thermally hardened) at 140 °C for 30 minutes, to thereby form an conductive layer having a thickness of 15 ⁇ .
• hydroxygallium phthalocyanine charge generating substance having a crystal structure showing intense peaks at Bragg angles (2 ⁇ 0.2°) of 7.5°, 9.9°, 16.3°, 18.6°, 25.1°, and 28.3° in CuKa characteristic X-ray diffraction were prepared.
• phthalocyanine were added 250 parts of cyclohexanone and 5 parts of a polyvinyl butyral (product name: S-LEC BX-1, manufactured by Sekisui Chemical Co., Ltd.), and the resultant mixture was dispersed by a sand mill apparatus using glass beads each having a diameter of 1 mm under a 23 ⁇ 3°C atmosphere for 1 hour. After the dispersion, 250 parts of ethyl acetate were added to prepare an application liquid for the charge generating layer. The application liquid for the charge generating layer was applied onto the intermediate layer by dip coating and dried at 100°C for 10 minutes, to thereby form a charge generating layer having a thickness of 0.26 ⁇ .
• a polyvinyl butyral product name: S-LEC BX-1, manufactured by Sekisui Chemical Co., Ltd.
• Example 1 the emulsion produced in Example 1 as an application liquid for a charge transporting layer was applied onto the charge generating layer by dip coating and heated at 130°C for 1 hour to form a charge transporting layer having a thickness of 10 ⁇ .
• an electrophotographic an electrophotographic
• Table 7 shows the emulsion used and conditions for the heating of a coat obtained by applying the emulsion.
• Electrophotographic photosensitive members were each produced by the same method as that of Example 79 except that: an emulsion shown in Table 7 was used for a charge transporting layer; and conditions for the heating of a coat obtained by applying the emulsion were changed as shown in Table 7. The evaluations of the photosensitive members were also performed by the same methods as those of Example 79. Table 7 shows the results.
• An organic electroluminescence device was produced as described below.
• ITO was formed into a film having a thickness of 100 nm on a glass substrate as a support by a sputtering method.
• the resultant was subjected to ultrasonic washing with acetone and isopropyl alcohol (IPA) sequentially.. After that, the resultant was subjected to boil washing with IPA and then dried. Further, the surface of the substrate was subjected to UV/ozone washing. Thus, an anode layer was obtained.
• IPA isopropyl alcohol
• an electron injecting layer having a thickness of 15 nm was formed by co-depositing bathophenanthroline and cesium carbonate from the vapor so that the concentration of cesium in the layer was 8.3 mass%. After that, silver (Ag) was formed into a film on the layer by a heating deposition method. Thus, a cathode layer having a
• a voltage of ⁇ V was applied between the anode layer and the cathode layer. As a result, it was confirmed that the device emitted light at 8,000 Cd/cm 2 .
• An organic electroluminescence device was produced by the same method as that of Example 157 except that N,N- di (naphthalene-l-yl ) -N, N-diphenylbenzidine (NPB) as a charge transporting substance was used instead of the compound (1-5) in Example 157.
• NBP N-diphenylbenzidine
• a voltage of 6 V was applied between the anode layer and the cathode layer. As a result, it was confirmed that the device emitted light at 9,000 Cd/cm 2 .
• Electrophotographic photosensitive members were each produced by the same method as that of Example 79 except that: an emulsion shown in Table 8 was used for a charge transporting layer; and conditions for the heating of a coat obtained by applying the emulsion were changed as shown in Table 8. The evaluations of the photosensitive members were also performed by the same methods as those of Example 79. Table 8 shows the results. Gentle
• Electrophotographic photosensitive members were each produced by the same method as that of Example 79 except that: a produced emulsion for a charge transporting layer was immediately used in dip coating without being left to stand still for 2 weeks; an emulsion shown in Table 8 was used; and conditions for the heating of a coat obtained by applying the emulsion were changed as shown in Table 8. The evaluations of the photosensitive members were also performed by the same methods as those of Example 79.
• Table 8 shows the results. Gentle irregularities were formed in each of the resultant electrophotographic
• Electrophotographic photosensitive members were each produced by the same method as that of Example 79 except that: an emulsion shown in Table 8 was used for a charge transporting layer; and conditions for the heating of a coat obtained by applying the emulsion were changed as shown in Table 8. The evaluations of the photosensitive members were also performed by the same methods as those of Example 79. Table 8 shows the results. Gentle
• Example 79 Example 1 130°C 60 minutes 0.55 urn A
• Example 80 Example 2 130°C 60 minutes 0.52 ym A
• Example 81 Example 3 130°C 60 minutes 0.53 urn A
• Example 82 Example 4 130°C 60 minutes 0.55 urn A
• Example 83 Example 5 130°C 60 minutes 0.51 urn A
• Example 84 Example 6 130°C 60 minutes 0.58 um A
• Example 85 Example 7 130°C 60 minutes 0.63 urn B
• Example 86 Example 8 130°C 60 minutes 0.57 ⁇ A
• Example 87 Example 9 130°C 60 minutes 0.63 urn B
• Example 88 Example 10 130°C 60 minutes 0.57 urn A
• Example 89 Example 11 130°C 60 minutes 0.58 um A
• Example 90 Example 12 130°C 60 minutes 0.68 ym B '
• Example 91 Example 13 130°C 60 minutes 0.67 um B
• Example 92 Example 14 130°C 60 minutes 0.63 um B
• Example ⁇ 93 Example 15 150°C 60 minutes 0.46 um A
• Example 94 Example 16 150°C 60 minutes 0.47 pm A
• Example 96 Example 18 130°C 60 minutes 0.55 um A
• Example 97 Example 19 130°C 60 minutes 0.57 um A
• Example 98 Example 20 150°C 60 minutes 0.45 um A
• Example 99 Example 21 130°C 60 minutes 0.55 um A
• Example 100 Example 22 130°C 60 minutes 0.54 um A
• Example 101 Example 23 130°C 60 minutes 0.50 um A
• Example 102 Example 24 130°C 60 minutes 0.50 um A
• Example 103 Example 25 130°C 60 minutes 0.55 um A
• Example 104 Example 26 130°C 60 minutes 0.53 um A
• Example 105 Example 27 130°C 60 minutes 0.57 um A
• Example 106 Example 28 130°C 60 minutes 0.57 um A
• Example 107 Example 29 130°C 60 minutes 0.59 um A
• Example 108 Example 30 130°C 60 minutes 0.60 um B
• Example 109 Example 31 130°C 60 minutes 0.59 um A
• Example 110 Example 32 130°C 60 minutes 0.58 um A
• Example 111 Example 33 130°C 60 minutes 0.53 um A
• Example 112 Example 34 130°C 60 minutes 0.51 um A
• Example 113 Example 35 130°C 60 minutes 0.55 um A
• Example 114 Example 36 130°C 60 minutes 0.50 um A
• Example 115 Example 37 150°C 40 minutes 0.45 um A
• Example 116 Example 38 130°C 90 minutes 0.57 um A
• Example 117 Example 39 130°C 60 minutes 0.52 um A
• Example 118 Example 40 130°C 60 minutes 0.58 um A
• Example 119 Example 41 130°C 60 minutes 0.52 um A
• Example 120 Example 42 130°C 60 minutes 0.56 um A
• Example 121 Example 43 130°C 60 minutes 0.56 um A
• Example 122 Example 44 130°C 40 minutes 0.51 um A
• Example 123 Example 45 130°C 60 minutes 0.57 ym A
• Example 124 Example 46 130°C 60 minutes 0.53 um A
• Example 125 Example 47 130°C 60 minutes 0.56 um A
• Example 126 Example 48 130°C 60 minutes 0.52 um A
• Example 127 Example 49 130°C 60 minutes 0.55 ym A
• Example 128 Example 50 130°C 60 minutes 0.57 um A
• Example 129 Example 51 130°C 60 minutes 0.55 ym A
• Example 130 Example 52 130°C 60 minutes 0.52 ym A
• Example 131 Example 53 130°C 60 minutes 0.60 ym B
• Example 132 Example 54 130°C 60 minutes 0.57 pm A
• Example 133 Example 55 130°C 60 minutes 0.51 pm A
• Example 134 Example 56 130°C 60 minutes 0.49 urn A
• Example 135 Example 57 130°C 60 minutes 0.44 urn A
• Example 136 Example 58 150°C 60 minutes 0.49 urn A
• Example 137 Example 59 130°C 60 minutes 0.50 urn A
• Example 138 Example 60 130°C 60 minutes 0.49 ⁇ A
• Example 139 Example 61 150°C 60 minutes 0.40 A
• Example 140 Example 62 130°C 60 minutes 0.45 urn A
• Example 141 Example 63 130°C 60 minutes 0.51 urn A
• Example 142 Example 64 130°C 60 minutes 0.49 urn A
• Example 143 Example 65 150°C 60 minutes 0.40 urn A
• Example 144 Example 66 130°C 60 minutes 0.47 pm A
• Example 145 Example 67 130°C 60 minutes 0.50 urn A
• Example 146 Example 68 130°C 60 minutes 0.48 m A
• Example 147 Example 69 130°C 60 minutes 0.48 urn A
• Example 148 Example 70 130°C 60 minutes 0.44 um A
• Example 149 Example 71 130°C 60 minutes 0.51 urn A
• Example 150 Example 72 130°C 60 minutes 0.50 um A
• Example 151 Example 73 130°C 60 minutes 0.45 um A
• Example 152 Example 74 130°C 60 minutes 0.44 um A
• Example 153 Example 75 130°C 60 minutes 0.52 um A
• Example 154 Example 76 130°C 60 minutes 0.49 pm A
• Example 155 Example 77 130°C 60 minutes 0.48 um A
• Example 156 Example 78 130°C 60 minutes 0.46 um A
• Example 213 Example 159 130°C 60 minutes 0.67 um B
• Example 214 Example 160 130°C 60 minutes 0.56 um A
• Example 215 Example 161 130°C 60 minutes 0.61 um B
• Example 216 Example 162 130°C 60 minutes 0.62 um B
• Example 217 Example 163 130°C 60 minutes 0.68 um B
• Example 218 Example 164 130°C 60 minutes 0.66 um B
• Example 219 Example 165 130°C 60 minutes 0.65 um B
• Example 220 Example 166 130°C 60 minutes 0.61 um B
• Example 221 Example 167 130°C 60 minutes 0.61 um B
• Example 222 Example 168 130°C 60 minutes 0.64 um B
• Example 223 Example 169 130°C 60 minutes 0.62 um B
• Example 224 Example 170 130°C 60 minutes 0.61 um B
• Example 225 Example 171 130°C 60 minutes 0.62 um B
• Example 226 Example 172 130°C 60 minutes 0.62 um B
• Example 227 Example 173 130°C 60 minutes 0.61 um B
• Example 228 Example 174 130°C 60 minutes 0.68 um B
• Example 229 Example 175 130°C 60 minutes 0.63 um B
• Example 230 Example 176 130°C 60 minutes 0.54 um A
• Example 231 Example 177 130°C 60 minutes 0.57 um A
• Example 232 Example 178 130°C 60 minutes 0.64 um B
• Example 233 Example 179 130°C 60 minutes 0.68 um B
• Example 234 Example 180 130°C 60 minutes 0.66 um B
• Example 235 Example 181 130°C 60 minutes 0.68 um B
• Example 236 Example 182 130°C 60 minutes 0.62 um B
• Example 237 Example 183 130°C 60 minutes 0.61 um B
• Example 238 Example 184 130°C 60 minutes 0.67 um B
• Example 239 Example 185 130°C 60 minutes 0.55 um A [0151] Table 7 (continued)
• Example 243 Example 240 130°C 60 minutes 0.54 urn A
• Example 244 Example 241 130°C 60 minutes 0.62 urn B
• Example 245 Example 242 130°C 60 minutes 0.56 urn A
• the emulsion formed only of the first liquid may be unable to provide sufficient coat uniformity as compared with that of the emulsion of the present invention containing both the first liquid and the second liquid even when the emulsion is not stored for a long time period.

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