WO1999059033A1 - Materiau extrude par fusion se pretant a l'elaboration de la couche de transfert d'une unite photosensible de dispositif de formation d'image - Google Patents

Materiau extrude par fusion se pretant a l'elaboration de la couche de transfert d'une unite photosensible de dispositif de formation d'image Download PDF

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Publication number
WO1999059033A1
WO1999059033A1 PCT/JP1999/002194 JP9902194W WO9959033A1 WO 1999059033 A1 WO1999059033 A1 WO 1999059033A1 JP 9902194 W JP9902194 W JP 9902194W WO 9959033 A1 WO9959033 A1 WO 9959033A1
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WO
WIPO (PCT)
Prior art keywords
melt
fluorine
extruded material
image forming
carbon black
Prior art date
Application number
PCT/JP1999/002194
Other languages
English (en)
French (fr)
Japanese (ja)
Inventor
Tatsuya Higuchi
Masami Kato
Original Assignee
Daikin Industries, Ltd.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Daikin Industries, Ltd. filed Critical Daikin Industries, Ltd.
Priority to KR1020007011660A priority Critical patent/KR20010034795A/ko
Priority to JP2000548777A priority patent/JP3743288B2/ja
Priority to EP99917146A priority patent/EP1079282A4/en
Publication of WO1999059033A1 publication Critical patent/WO1999059033A1/ja

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Classifications

    • GPHYSICS
    • G03PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03GELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G15/00Apparatus for electrographic processes using a charge pattern
    • G03G15/14Apparatus for electrographic processes using a charge pattern for transferring a pattern to a second base
    • G03G15/16Apparatus for electrographic processes using a charge pattern for transferring a pattern to a second base of a toner pattern, e.g. a powder pattern, e.g. magnetic transfer
    • GPHYSICS
    • G03PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03GELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G15/00Apparatus for electrographic processes using a charge pattern
    • G03G15/14Apparatus for electrographic processes using a charge pattern for transferring a pattern to a second base
    • G03G15/16Apparatus for electrographic processes using a charge pattern for transferring a pattern to a second base of a toner pattern, e.g. a powder pattern, e.g. magnetic transfer
    • G03G15/1665Apparatus for electrographic processes using a charge pattern for transferring a pattern to a second base of a toner pattern, e.g. a powder pattern, e.g. magnetic transfer by introducing the second base in the nip formed by the recording member and at least one transfer member, e.g. in combination with bias or heat
    • G03G15/167Apparatus for electrographic processes using a charge pattern for transferring a pattern to a second base of a toner pattern, e.g. a powder pattern, e.g. magnetic transfer by introducing the second base in the nip formed by the recording member and at least one transfer member, e.g. in combination with bias or heat at least one of the recording member or the transfer member being rotatable during the transfer
    • G03G15/1685Structure, details of the transfer member, e.g. chemical composition

Definitions

  • the present invention relates to a melt-extrusion material suitable for forming a transfer layer of a photosensitive section of an image forming apparatus and a transfer belt of a photosensitive section formed by using the same.
  • a melt-extrusion material suitable for forming a transfer layer of a photosensitive section of an image forming apparatus and a transfer belt of a photosensitive section formed by using the same.
  • Fluororesin is excellent in chemical lubrication, thermal stability, surface lubrication, electrical properties, mechanical properties, and abrasion resistance. Widely used in material carriers and image forming units.
  • the fluororesin composition is an insulator with a volume-specific resistivity exceeding 10 16 ⁇ -cm, and the pressurized roller in the electronic copying machine ⁇ In the mouth, etc., static electricity may cause paper sheets to be adsorbed, and toner powder to be absorbed or scattered may cause trouble. It was.
  • a conductive material into a fluororesin composition.
  • the conductive material include carbon black, graphite powder, carbon material such as carbon fiber, and metal powder.
  • conductive belts are frequently used.
  • a thermoplastic resin in which a conductive carbon black is combined is generally used. This is formed into a film and processed to form a belt.
  • a simple belt what is extruded and formed into a cylindrical film, and this cylindrical file is cut in a direction of a water square, is known as a simple belt.
  • thermoplastic resins are used as required.
  • fluorine-based polymers are superior to other thermoplastic resins in terms of flame retardancy, durability, and filming resistance (toner releasability). Therefore, it is frequently used.
  • the resistance value of the conductive belt in a multi-function printer, a printer, a facsimile machine, etc. using a fluorine-based polymer conductive belt increases over time. There was a problem that the image was degraded due to a drastic drop. For example, when the belt is used for an intermediate transfer belt such as a duplicator, the toner is electrically pulled to the belt surface. It must be charged in order to generate a high voltage repeatedly, for example by corona discharge.
  • the high voltage causes the fluorine-based polymer belt to have a gradual decrease in the resistance value, and as a result, The amount of transfer of the toner to the camera is reduced, which has an adverse effect on the image.
  • This phenomenon occurs on the fluorine-containing polymer belt because of the separation of the conductive filler from the fluorine-containing polymer and the interface between the conductive filler and the fluorine-containing polymer. It is thought that a trap in the conductive carrier due to a crystal defect inside the polymer causes the resistance to decrease due to the space charge limiting current. It is.
  • so-called semi-conductive rollers and belts such as charged rollers and belts, transfer rollers, and image openings in electronic duplicators.
  • a specific range of conductivity is required. Specifically, mouth - volume is have you in La Ya bell door-specific resistivity of force "0 8 ⁇ : 1 0 1 3 ⁇ ⁇ cm need to range Ru is co-emissions collected by filtration Lumpur is is there .
  • the present invention relates to a melt-extrusion material suitable for forming a transfer layer of a photosensitive portion of an image forming apparatus, and in particular, a volume-specific resistivity control that is easy and non-viscous Melt extrusion material made of fluorine-containing resin with excellent adhesion, smoothness and strength, and transfer using it Disclosure of the invention aimed at providing beryrets
  • the present invention relates to a composition
  • a composition comprising (A) at least a part of a fluorinated filler and (B) a fluorine-containing thermoplastic resin. and Oh one, e la Re that the front surface of the body volume-specific resistance ratio of the film is 10 8 ⁇ 10 1 3 ⁇ ⁇ cm, vs. water contact touch corner 96 degrees or more on your good beauty the film tensile Suitable for forming a transfer layer of the light-sensitive part of an image forming apparatus characterized by being a composition having a strength of 400 kgf / cm 2 or more at 25 ° C.
  • the present invention relates to a melt-extruded material and a transfer belt formed by using the material.
  • the melt-extruded material of the present invention contains at least a partly fluorinated filler (A) and a filler.
  • the (A) component consisting of a fluorine-containing thermoplastic resin (B) and at least a part of which is a fluorinated filler, is a force pump.
  • carbon materials such as rack, carbon fiber, petroleum coke, and graphite powder are fluorinated.
  • the fluorination power obtained by fluorinating a carbon book is a carbon black, especially a fluorine against a carbon atom.
  • Fluorinated carbon black with an atomic ratio FZC of 0.1 or more and less than 1.0, particularly 0.1 or more and less than 0.5 is preferable.
  • One of the problems with the carbon materials is that the rate of change of resistance with respect to the amount of connection is extremely large, and the control of the conductive material is very large. Difficulty and uneven distribution of the fluorinated carbon black due to the structure that has been developed. The problem that the resulting composition becomes hard remains. If the F / C force is greater than 1.0, it is not possible to impart the desired conductivity to the composition.
  • FZC is measured as follows. Wrap the fluorinated carbon black in filter paper together with the flame retardant Na 2 O 2 and polyethylene film, and fill with oxygen. Combustion in a hermetically closed flask, the generated hydrogen fluoride is converted into a fluoride ion meter (Olyon Corporation: Ion Analyzer 901). Measure according to the standard method. This value is used to calculate the fluorine content. The FZC is calculated based on the obtained fluorine content.
  • the carbon black (A) is composed mainly of poly (carbon monofluoride), and the average of the carbon black (A) is the average.
  • a ⁇ ⁇ force block is a fluorine gas that has been fluorine-fluorinated. I like it. Fluorination obtained from carbon materials with an average particle size of more than 50 ⁇ m, for example, petroleum coke, graphite powder, carbon fiber, etc.
  • the carbon black must have a large amount to impart conductivity and non-adhesion to the resin, and the resulting composition must have a rough surface. The tendency is to cause problems such as an increase in temperature, deterioration in mechanical strength, and unevenness in resistivity.
  • Suitable as a carbon material for the fluorinated carbon black (A) is a carbon black having the above-mentioned average particle size.
  • the carbon black is, for example, a rubber fan black (for example, Asahi # 55 manufactured by Asahi Rikiichi Bonn Co., Ltd.). ), Color channel black (for example, Carbon Carbon Revenue 7000), Thermal Black (Colonia Carbon Seno, 'Carbon MT-C1), etc. Commercially available products can be used.
  • Carbon blacks especially those commonly referred to as conductive carbon blacks.
  • Conductive mosquitoes over Bonn Bed rack is had average particle size of small flat (average particle diameter 0. 1 mu m or less under flat), have come front surface product is large (N 2 surface area 50 m 2 / g or more), the structure is developed (P and oil amount lOOccZg or more), the amount of impurities is small (ash content is less than 0.1%), and the grapha It is defined by the fact that it is advancing, and it is possible to impart conductivity to the material with a relatively small amount of compounding. Therefore, it is widely used.
  • ketchbox EC ketchbox EC-600 JD (hereinafter, ketchbox black).
  • International Co., Ltd. Black Pearls 200, Vulcan XC-72, CSX-99 (hereafter referred to as Black Denka Black Co., Ltd. (Electrical Chemistry Engineering Co., Ltd.), Conductex 950 (Columbia Carbon Co., Ltd.), etc. Is on the market.
  • the fluorine black carbon black (A) used in the present invention is prepared by subjecting such a carbon material to a temperature in the range of 200 to 600 ° C. More preferably, it is obtained by contacting with fluorine gas at a temperature in the range of 300 to 500 ° C. At a reaction temperature lower than this range, the fluorination reaction progresses slowly, the degree of fluorination is hard to increase, and the thermal stability is not sufficient. However, problems such as the non-adhesiveness and lubricity of the fluorinated carbon black cannot be achieved. Conversely, if the reaction temperature is higher than this range, the pyrolysis reaction is likely to occur, and the The yield rate of fluorine carbon black will be reduced. Also, it is necessary to pay close attention to the fact that a sudden thermal decomposition reaction may occur and cause an explosion.
  • the fluorine gas used for the reaction may be diluted with an inert gas such as nitrogen, argon, helium, tetrafluorocarbon, or the like. In addition, it may contain hydrogen fluoride. Also, the reaction can be carried out at normal pressure, but it does not work at all even if the pressure is reduced or applied.
  • reaction time In addition to the above conditions, the reaction time, fluorine gas flow rate, etc., depend on the reactivity of the raw material carbon material with fluorine and the desired FZC (containing fluorine). The amount should be adjusted accordingly.
  • a feature of the present invention is to provide a fluorine-containing thermoplastic resin material which can be melt-extruded and formed.
  • rubber materials such as fluorine rubber and silicone rubber have been used in this field, but materials mainly made of these rubbers are used. Cannot be melt extruded.
  • Fluoro-containing thermoplastics include tetrafluoroethylene (TFE) and at least one other species that can be co-polymerized with it. Ren-unsaturated monomers (eg, ethylene, propylene, etc., olefins, hexafluoropropylene, vinylidene) Fluoride, black mouth trifluorene, vinyl fluoride, etc., gen- erated olefins, pamphlets Copolymers with fluoroalkyl vinyl ethers, etc.), polyclonal trifluoroethylene, polyvinylidene Orid etc. are exposed.
  • a particularly preferred fluorine-containing thermoplastic resin is a fluorine-containing thermoplastic resin having a hydrogen atom.
  • the plastic resin is distinguished from the point that high strength is obtained and the point that it is excellent in additivity.
  • ethylene-tetrafluoroethylene copolymer ETFE
  • PVdF polyvinylidene fluoridation
  • vinylidene Fluorofluorohexyl copolymers are preferred because of their high strength and high potency.
  • fluorine-containing thermoplastic resins they have superior heat resistance, non-adhesion, water and oil repellency, lubricity, and chemical resistance compared to general-purpose resins. The effect is obtained that a composition having the following is obtained.
  • general-purpose resins include, for example, polyether ether ketone, thermoplastic thermoplastic polyimide, polyethylene naphthalate, and the like.
  • Polybutyrene, evening rate, polyethersulfone, polysulfone, polycarbonate, polyaryt, poly Non-fluorothermoplastic resins, such as polyethylene terephthalate and polyethernitrile, can be used.
  • the composition ratio of the component (A) and the component (B) is 1/99 to 20Z80 (weight ratio; the same applies hereinafter).
  • the component (B) may be mixed with the non-fluorine-based thermoplastic resin in such an amount that the effect of the present invention is not impaired.
  • the features of the melt-extrusion material of the present invention are that it has good extrusion moldability even without adding a plasticizer, and it does not require the addition of a surfactant. The point is that stable semiconductivity can be obtained. Therefore, in the past, leaching (bleeding) was a problem and was a source of contamination. And the addition of a fluorine-based surface active agent can be eliminated.
  • composition of the present invention can be mixed and prepared by a usual method, for example, a simple method.
  • a mixer such as a kneader
  • the mixture is further mixed using a melting and kneading device such as a twin screw extruder to form a pellet.
  • the pellets obtained by the extruder are used to form the desired shape, for example, a belt, plate, film, etc. It is formed.
  • the melt-extrusion material of the present invention has physical properties suitable as a material for forming a transfer layer of a photosensitive portion of an image forming apparatus.
  • the coatings (tubes, films, etc.) obtained by melting and extruding the material of the present invention have the following physical properties.
  • the surface has a specific volume resistivity of 10 8 to 10 13 Q * cm, preferably l O l O ⁇ Q 'cm. As long as it is within this range, excellent toner transfer will be performed.
  • the ratio of the maximum value and the minimum value of the volume specific resistivity on the same coating surface is 10 or less, and the semiconductivity is uniform, so that dielectric breakdown does not occur.
  • the contact angle with water is 96 degrees or more, preferably 98 degrees or more. When the contact angle with water is large, the non-adhesiveness is good.
  • the surface roughness (Ra) force is preferably 5 ⁇ or less, and more preferably 0.5 ⁇ or less.
  • a smooth surface having a small surface roughness (R a) has little toner residue and is excellent in terms of image formation.
  • the transfer belt to which the present invention is applied takes a large amount of tension when rotating at high speed.
  • transfer belts satisfying the characteristics of (1), (2), and (4) above and imparting a large tensile strength have been conventionally used. Rather, it has been achieved for the first time in the present invention.
  • the material of the present invention can provide various shaped articles by the melt extrusion molding method. For example, it can be formed into a film, a tube, a plate, a belt or the like. Such a melt extruded product cannot be homogeneous unless it is excellent in melt formability. In this regard, if the fluorinated force is combined with a bon black, as described above, it is melted due to the structure. The melt viscosity becomes remarkably large, the melt-kneading becomes insufficient, and the dispersion becomes uneven.
  • the material of the present invention is preferably within a range where melt flow rate (MFR), which is one of the indicators of melt formability, is acceptable (0.5 gZlO or more). ETFE: 297 ° C, PVdF: 230 ° C, load 5 kg) ⁇ It is dispersible (meltability) together with its melt formability. Is also good.
  • the present invention also relates to a transfer belt for a photosensitive section of an image forming apparatus.
  • the image forming apparatus used in the present invention may be an electronic photocopier, a facsimile machine, a laser printer, or a laser printer. Not limited to them, but based on electrostatic duplication Includes equipment for transferring toner.
  • a charging roller, a current image roller, and a transfer belt which are usually semiconductive rollers, are usually used. Or roller) Powerful.
  • the transfer belt usually has an endless transfer belt.
  • the transfer paper By pressing the transfer paper against the photosensitive drum with three rollers, the toner image on the photosensitive drum is transferred to the transfer paper. I will do it.
  • Such a transfer belt is a single endless belt (typically 50 to 250 m thick) or a transfer layer (thickness) on a heat-resistant resin woven fabric. (About 10 to 50 / im), but the transfer belt of the present invention can be applied to those conventional structures. It is a thing.
  • melt-extrusion material of the present invention is useful not only as a transfer belt but also as a resistor layer for a transfer roller, a charged roller, a current image roller, and the like. It is.
  • a conductive elastic layer is formed first on a conductive support.
  • the material for the conductive elastic layer is not particularly limited, and may be silicone rubber, ethylene propylene rubber, or epoxy rubber.
  • Conductive powders and conductive fibers are contained in composite rubber such as chlorohydrin rubber, nitrile rubber, and urethane rubber. Powders, carbon fibers, etc.), and has a volume-specific resistivity of 10 5 Q'cm or less. Is less than 10 3 Q'cm and has a rubber hardness (JIS A) force S in the range of 20 to 50 degrees, preferably 25 to 40 degrees. .
  • a plasticizer or surface active agent for the purpose of resistance adjustment or rubber hardness adjustment. Absent . This means that these chemicals ooze out over time, contaminating the surface of photosensitizers and the like, and toner filming on the roller surface. This is a cause of the occurrence of the
  • the material of the conductive support is not particularly limited, and the alloy mainly composed of aluminum or aluminum is used. Can use stainless steel.
  • the melt-extrusion material of the present invention is formed into a tube-like film by a usual melt-extrusion molding method. It may be stretched or heat-shrinkable if necessary, but usually does not have to be stretched or heat-shrinkable.
  • the thickness of such a tube must be in the range of 0.01 to 0.15 mm, and it is preferable to deviate from this value. No part rollers are available.
  • a core metal and a tube made of the melt-extrusion material according to the present invention are arranged inside the tubular molded body with a space between them. It is arranged so that the inner surface of the cylindrical molded body and the outer surface of the tube are in contact with each other, and the material for the conductive elastic layer is flowed through the above-mentioned space.
  • the roller for the photosensitive portion of the present invention can be obtained by vulcanizing it if necessary and vulcanizing it if necessary. Of course, it is necessary to take out the roller part, including the coated tube, from the tubular molded body when necessary.
  • a conductive elastic layer may be prepared in advance, and the surface thereof may be covered with a tube to be placed in the present invention. In this case, it is better to use a heat-shrinkable tube.
  • the melt-extrusion material of the present invention is applied to various types of rollers or belts of the photosensitive section of an image forming apparatus, and particularly to a transfer belt which requires a high strength. Good for rooting.
  • the part indicates the weight part.
  • Fluorine black (denka black manufactured by Electrochemical Engineering Co., Ltd .; average particle size: 0.04 m) is fluorine-filtered to obtain an FZC of 0.1. Fluorinated carbon black has been created.
  • the fluoridation power of 10 parts of the black block and 90 parts of the ETFE are 90 parts.
  • the mixture is melted at 300 ° C in a twin-screw extruder (Laboplasty mill made by Toyo Seiki Co., Ltd.). They were kneaded, extruded, and pelleted. This pellet is extruded into a film (300 °) with an extruder (30 ⁇ single-axis extruder manufactured by Tanabe Plastics Co., Ltd.). C), A film with a thickness of 150 ⁇ was produced.
  • a fan measurement cell (Registration Channel No.R12702A) manufactured by Advanst Co., Ltd. and a resistance meter (Digit Meter) Measure using a tall ultra-high resistance meter R 8340 A).
  • Ra is the center average roughness specified in JIS B 0601-1982.
  • melt extrusion rate (ETFE 297 ° C, PV d F: 230 ° C, load 5kg). The results are shown in Table 1.
  • Example 1 a film was produced by melt-extrusion molding using ETFE alone without combining a fluorine-containing carbon black film, and measuring the properties of the film. Specified. Table 1 shows the results.
  • Example 1 in place of the fluorinated carbon black, a non-fluorinated raw material carbon black (manufactured by Denki Kagaku Kogyo Co., Ltd.) The average particle size is 0.04 ⁇ m).
  • the blended amounts shown in Table 1 were melt-extruded to form films, and the physical properties were measured. Table 1 shows the results.
  • the mixture in the amounts shown was melt-extruded to produce a film, and each physical property was measured. The results are shown in Table 1.
  • melt-extrusion material of the present invention is excellent in melt formability (MFR), and the melt extruded material is also a fluoropolymer.
  • the change in the volume specific resistivity is small even when the amount of the mixed metal is changed (Comparing Examples 1 and 2, 3 and 4, and 5 and 6), and the non-adhesive property (water contact) It provides molded products that have excellent strength and smoothness (surface roughness) and have sufficient strength and are suitable for transfer belts or rollers in the photosensitive area.

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Electrostatic Charge, Transfer And Separation In Electrography (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Extrusion Moulding Of Plastics Or The Like (AREA)
PCT/JP1999/002194 1998-05-13 1999-04-26 Materiau extrude par fusion se pretant a l'elaboration de la couche de transfert d'une unite photosensible de dispositif de formation d'image WO1999059033A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
KR1020007011660A KR20010034795A (ko) 1998-05-13 1999-04-26 화상형성장치의 감광부의 전사층의 형성에 적합한용융압출재료
JP2000548777A JP3743288B2 (ja) 1998-05-13 1999-04-26 画像形成装置の転写層用溶融押出材料
EP99917146A EP1079282A4 (en) 1998-05-13 1999-04-26 MATERIAL EXTRUDED BY MELTING SUITABLE FOR DEVELOPING THE TRANSFER LAYER OF A PHOTOSENSITIVE UNIT OF IMAGE FORMING DEVICE

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP13081198 1998-05-13
JP10/130811 1998-05-13

Publications (1)

Publication Number Publication Date
WO1999059033A1 true WO1999059033A1 (fr) 1999-11-18

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PCT/JP1999/002194 WO1999059033A1 (fr) 1998-05-13 1999-04-26 Materiau extrude par fusion se pretant a l'elaboration de la couche de transfert d'une unite photosensible de dispositif de formation d'image

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EP (1) EP1079282A4 (ko)
JP (1) JP3743288B2 (ko)
KR (1) KR20010034795A (ko)
WO (1) WO1999059033A1 (ko)

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JP2003084519A (ja) * 2001-09-13 2003-03-19 Daikin Ind Ltd 押出成形用フッ素系組成物、感光部用成形物製造方法及び感光部用成形物

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US20030096917A1 (en) * 2001-08-23 2003-05-22 Sumitomo Rubber Industries, Ltd. Polymer composition for conductive roller, polymer composition, conductive roller, and conductive belt
KR101157321B1 (ko) * 2008-03-06 2012-06-15 코오롱인더스트리 주식회사 중간전사벨트 및 그 제조방법
JP6414110B2 (ja) * 2015-04-28 2018-10-31 京セラドキュメントソリューションズ株式会社 画像形成装置
JP6406295B2 (ja) * 2015-04-28 2018-10-17 京セラドキュメントソリューションズ株式会社 画像形成装置
JP6597648B2 (ja) * 2017-01-13 2019-10-30 トヨタ自動車株式会社 リチウムイオン二次電池の製造方法

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JPH0954506A (ja) * 1995-06-06 1997-02-25 Canon Inc 画像形成装置及び中間転写体
JPH09169917A (ja) * 1995-12-18 1997-06-30 Ricoh Co Ltd 帯電防止性樹脂組成物
JPH09230716A (ja) * 1995-12-21 1997-09-05 Canon Inc 像担持ベルトとこのベルトを用いた画像形成装置
JPH09269676A (ja) * 1996-03-29 1997-10-14 Tokai Rubber Ind Ltd プラスチック無端ベルト
JPH09324128A (ja) * 1996-06-05 1997-12-16 Daikin Ind Ltd フッ化カーボン組成物、塗料および画像形成部材ならびに複合材料および製法
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JP3743288B2 (ja) 2006-02-08
KR20010034795A (ko) 2001-04-25
EP1079282A1 (en) 2001-02-28
EP1079282A4 (en) 2004-11-17

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