JPH023071A - Process for treating photosensitive body - Google Patents
Process for treating photosensitive bodyInfo
- Publication number
- JPH023071A JPH023071A JP15289688A JP15289688A JPH023071A JP H023071 A JPH023071 A JP H023071A JP 15289688 A JP15289688 A JP 15289688A JP 15289688 A JP15289688 A JP 15289688A JP H023071 A JPH023071 A JP H023071A
- Authority
- JP
- Japan
- Prior art keywords
- amorphous carbon
- carbon film
- carbene
- substrate
- photoreceptor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
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- 108091008695 photoreceptors Proteins 0.000 claims description 34
- 239000000126 substance Substances 0.000 claims description 18
- 238000006116 polymerization reaction Methods 0.000 claims description 15
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 abstract description 33
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- 125000005843 halogen group Chemical group 0.000 abstract description 13
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- HZVOZRGWRWCICA-UHFFFAOYSA-N methanediyl Chemical compound [CH2] HZVOZRGWRWCICA-UHFFFAOYSA-N 0.000 abstract description 5
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- QBNFBHXQESNSNP-UHFFFAOYSA-N humulene Natural products CC1=CC=CC(C)(C)CC=C(/C)CCC1 QBNFBHXQESNSNP-UHFFFAOYSA-N 0.000 description 1
- 229910000042 hydrogen bromide Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 229910000043 hydrogen iodide Inorganic materials 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- INQOMBQAUSQDDS-UHFFFAOYSA-N iodomethane Chemical compound IC INQOMBQAUSQDDS-UHFFFAOYSA-N 0.000 description 1
- 239000001282 iso-butane Substances 0.000 description 1
- 150000002561 ketenes Chemical class 0.000 description 1
- 229940087305 limonene Drugs 0.000 description 1
- 235000001510 limonene Nutrition 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- AUHZEENZYGFFBQ-UHFFFAOYSA-N mesitylene Substances CC1=CC(C)=CC(C)=C1 AUHZEENZYGFFBQ-UHFFFAOYSA-N 0.000 description 1
- 125000001827 mesitylenyl group Chemical group [H]C1=C(C(*)=C(C([H])=C1C([H])([H])[H])C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 229940102396 methyl bromide Drugs 0.000 description 1
- PYLWMHQQBFSUBP-UHFFFAOYSA-N monofluorobenzene Chemical compound FC1=CC=CC=C1 PYLWMHQQBFSUBP-UHFFFAOYSA-N 0.000 description 1
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- QYSGYZVSCZSLHT-UHFFFAOYSA-N octafluoropropane Chemical compound FC(F)(F)C(F)(F)C(F)(F)F QYSGYZVSCZSLHT-UHFFFAOYSA-N 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- BEZDDPMMPIDMGJ-UHFFFAOYSA-N pentamethylbenzene Chemical compound CC1=CC(C)=C(C)C(C)=C1C BEZDDPMMPIDMGJ-UHFFFAOYSA-N 0.000 description 1
- RGSFGYAAUTVSQA-UHFFFAOYSA-N pentamethylene Natural products C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 description 1
- YWAKXRMUMFPDSH-UHFFFAOYSA-N pentene Chemical compound CCCC=C YWAKXRMUMFPDSH-UHFFFAOYSA-N 0.000 description 1
- 229960004065 perflutren Drugs 0.000 description 1
- 230000001443 photoexcitation Effects 0.000 description 1
- 230000036211 photosensitivity Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 229920001230 polyarylate Polymers 0.000 description 1
- 229920005668 polycarbonate resin Polymers 0.000 description 1
- 239000004431 polycarbonate resin Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- MWWATHDPGQKSAR-UHFFFAOYSA-N propyne Chemical group CC#C MWWATHDPGQKSAR-UHFFFAOYSA-N 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 101150050201 sec11 gene Proteins 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- PJANXHGTPQOBST-UHFFFAOYSA-N stilbene Chemical compound C=1C=CC=CC=1C=CC1=CC=CC=C1 PJANXHGTPQOBST-UHFFFAOYSA-N 0.000 description 1
- 235000021286 stilbenes Nutrition 0.000 description 1
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 1
- UOHMMEJUHBCKEE-UHFFFAOYSA-N tetramethylbenzene Natural products CC1=CC=C(C)C(C)=C1C UOHMMEJUHBCKEE-UHFFFAOYSA-N 0.000 description 1
- FLTJDUOFAQWHDF-UHFFFAOYSA-N trimethyl pentane Natural products CCCCC(C)(C)C FLTJDUOFAQWHDF-UHFFFAOYSA-N 0.000 description 1
- AAAQKTZKLRYKHR-UHFFFAOYSA-N triphenylmethane Chemical compound C1=CC=CC=C1C(C=1C=CC=CC=1)C1=CC=CC=C1 AAAQKTZKLRYKHR-UHFFFAOYSA-N 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- VMYXUZSZMNBRCN-UHFFFAOYSA-N α-curcumene Chemical compound CC(C)=CCCC(C)C1=CC=C(C)C=C1 VMYXUZSZMNBRCN-UHFFFAOYSA-N 0.000 description 1
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
- G03G5/14—Inert intermediate or cover layers for charge-receiving layers
- G03G5/147—Cover layers
- G03G5/14704—Cover layers comprising inorganic material
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Photoreceptors In Electrophotography (AREA)
Abstract
Description
【発明の詳細な説明】 産業上の利用分野 本発明は感光体の処理方法に関する。[Detailed description of the invention] Industrial applications The present invention relates to a method of processing a photoreceptor.
従来技術および課題
種々の有機化合物がプラズマ重合法により膜状に形成さ
れることが知られており、該膜は例えば有機系感光体の
電荷輸送層、電荷発生層、表面保護層、あるいはアンダ
ーコート層等として種々応用研究開発がなされている。Prior Art and Problems It is known that various organic compounds are formed into films by plasma polymerization, and these films can be used, for example, as charge transport layers, charge generation layers, surface protection layers, or undercoats of organic photoreceptors. Various applied research and developments have been carried out as layers, etc.
プラズマ重合法により形成された有機膜は、通常非晶質
であり（以下、このような膜を［非晶質炭素膜という）
、以下のような特徴を有する：■高硬度である：鉛筆硬
度（Ｊ Ｉｓ−に−５４００）３Ｈ以上のものが容易に
得られる。Organic films formed by plasma polymerization are usually amorphous (hereinafter, such films are referred to as amorphous carbon films).
, has the following characteristics: ■High hardness: Pencil hardness (JIs-5400) of 3H or higher can be easily obtained.
◎被コート材、特に有機質材との密着性がよい。◎Good adhesion to coated materials, especially organic materials.
Ｏ耐溶剤性、耐酸性、耐アルカリ性がよい。Good solvent resistance, acid resistance, and alkali resistance.
＠透光性に秀れている。@Excellent translucency.
■摩擦係数が低く、耐摩耗性に優れている。■Low coefficient of friction and excellent wear resistance.
しかし、上記したごとく良好な特性を有する非晶質炭素
数膜は、残留ラジカル、未結合手やウィークポンド等の
ためある程度活性な状態にあるので、長期間にわたり自
然放置しておくと、空気中の酸素や水分の付着等を受は
膜特性の劣化がおこる。また、非晶質炭素膜を応用した
有機系感光体は、電子写真複写工程の１つである帯電工
程中、コロナ放電等を受けるが、膜中の残留ラジカル、
未結合手やウィークポンド等を有する部分にコロナ放電
等によりさらに水分等が付着しやすくなり、画像流れ、
表面電位の低下による画像濃度の低下等の感光体の特性
劣化が生じる。その現象は高湿環境下になればなる程発
生しやすい。However, as mentioned above, amorphous carbon films with good properties are in a somewhat active state due to residual radicals, dangling bonds, weak pounds, etc., so if left for a long period of time, they will not be exposed to air. If the membrane is exposed to adhesion of oxygen or moisture, the membrane properties will deteriorate. In addition, organic photoreceptors using amorphous carbon films are subjected to corona discharge, etc. during the charging process, which is one of the electrophotographic copying processes, but residual radicals in the film,
Due to corona discharge, etc., moisture tends to adhere to areas with dangling bonds, weak bonds, etc., resulting in image blurring and
Due to a decrease in surface potential, characteristics of the photoreceptor such as a decrease in image density occur. The more humid the environment, the more likely this phenomenon will occur.
本発明は上記したような非晶質炭素膜の経時的特性劣化
を防止し、長期間にわたって感光体特性に優れ、良好な
画像を形成することを可能とする感光体の処理方法を提
供することを目的とする。The present invention provides a photoreceptor processing method that prevents the deterioration of the characteristics of an amorphous carbon film over time as described above, provides excellent photoreceptor characteristics over a long period of time, and makes it possible to form good images. With the goal.
課題を解決するための手段
ｔなわち本発明は、プラズマ重合法にＬり形成される非
晶質炭素膜を有する感光体の製造方法において、該非晶
質炭素膜をカルベン形成物質で処理する工程を含むこと
を特徴とする感光体処理方法に関する。Means for Solving the Problems That is, the present invention provides a method for manufacturing a photoreceptor having an amorphous carbon film formed by plasma polymerization, which includes a step of treating the amorphous carbon film with a carbene-forming substance. The present invention relates to a method for processing a photoreceptor, the method comprising:
非晶質炭素膜は、例えば、気相状態の分子を減圧下で放
電分解し１、発生したプラズマ雰囲気中に含まれる活性
中性種あるいは荷電種を基板上に拡散、電気力、あるい
は磁気力等により誘導し、基板上での再結合反応により
固相として堆積させる、所謂プラズマ重合反応から生成
させる。For example, an amorphous carbon film is produced by decomposing molecules in a gas phase by discharge under reduced pressure (1), and then diffusing active neutral species or charged species contained in the generated plasma atmosphere onto a substrate, using electric or magnetic force. It is generated from a so-called plasma polymerization reaction, in which the polymer is induced as a solid phase by a recombination reaction on a substrate.
非晶質炭素膜形成に使用する炭化水素の相状態は常温常
圧において必ずしも気相である必要は無く、加熱或いは
減圧等により溶融、蒸発、昇華等を経て気化し得るもの
であれば、液相でも固相でも使用可能である。該炭化水
素としては、例えば、飽和炭化水素、不飽和炭化水素、
脂環式炭化水素、芳香族炭化水素等が用いられる。The phase state of the hydrocarbon used to form an amorphous carbon film does not necessarily have to be a gas phase at room temperature and normal pressure; it can be a liquid as long as it can be vaporized through melting, evaporation, sublimation, etc. by heating or reduced pressure. Either phase or solid phase can be used. Examples of the hydrocarbons include saturated hydrocarbons, unsaturated hydrocarbons,
Alicyclic hydrocarbons, aromatic hydrocarbons, etc. are used.
使用可能な炭化水素には種類が多いが、飽和炭化水素と
しては、例えば、メタン、１タン、プロパン、ブタン、
ペンタン、ヘキサン、ヘプタ〕／、オクタン、イソブタ
ン、インペンタン、ネオペンタン、イソヘキサン、ネオ
ヘキサン、ジメチルブタン、メチルヘキサン、エチルペ
ンタン、ジメチルペンクン、トリブタン、メチルへ、ブ
タン、ジメチルブタン、トリメチルペンタン、イソナノ
ン等が用いられる。不飽和炭化水素としては、例えハ、
エチレン、プロピレン、イソブチレン、ブテン、ペンテ
ン、メチルブテン、ヘキセン、テトラメチルエチレン、
ヘプテン、オクテン、アレン、メチルアレン、ブタジェ
ン、ペンタジェン、ヘキサジエン、シクロペンタジェン
、オフメン、アロシメン、ミルセン、ヘキサトリエン、
アセチレン、ジアセチレン、メチルアセチレン、ブチン
、ペンチン、ヘキシン、ヘプチン、オクチン等が用いら
れる。脂環式炭化水素としては、例えば、シクロプロパ
ン、シクロブタン、〜シクロペンクン、シクロヘキサン
、シクロへブタン、シクロオクタン、シクロプロペン、
シクロブテン、シクロペンテン、シクロヘキセン、／ク
ロヘプテン、シクロオクテン、リモネン、テルビルン、
７エランドレン、シルベストレン、ツエン、カレン、ピ
不：／、ポルニレン、カンフエン、フェンチェン、シク
ロブタンチエン、トリンクレン、ビサポレン、ジンギベ
レン、クルクメン、フムレン、カジ不ンセスキベ二ヘン
、セリ不ン、カリオフィレン、サンタレン、セドレン、
カンホレン、フィロクラテン、ポドカルブレン、ミレン
等が用いられる。芳香族炭化水素としては、例えば、ベ
ンゼン、トルエン、キシレン、ヘミメリテン、プソイド
クメン、メシチレン、プレニテン、インジュレン、ジュ
レン、ペンタメチルベンゼン、ヘキサメチルベンゼン、
エチルベンゼン、プロピルベンゼン、クメン、スチレン
、ビフェニル、テルフェニル、ジフェニルメタン、トリ
フェニルメタン、ジベンジル、スチルベン、インデン、
ナフタリン、テトラリン、アントラセン、フェナントレ
ン等が単独であるいは混合して用いられる。There are many types of hydrocarbons that can be used, but examples of saturated hydrocarbons include methane, monotane, propane, butane,
Pentane, hexane, heptane]/, octane, isobutane, impentane, neopentane, isohexane, neohexane, dimethylbutane, methylhexane, ethylpentane, dimethylpenkune, tributane, methylpentane, butane, dimethylbutane, trimethylpentane, isonanone, etc. is used. Examples of unsaturated hydrocarbons include C,
Ethylene, propylene, isobutylene, butene, pentene, methylbutene, hexene, tetramethylethylene,
Heptene, octene, allene, methylalene, butadiene, pentadiene, hexadiene, cyclopentadiene, ofmene, allocimene, myrcene, hexatriene,
Acetylene, diacetylene, methylacetylene, butyne, pentyne, hexyne, heptyne, octyne, etc. are used. Examples of alicyclic hydrocarbons include cyclopropane, cyclobutane, ~cyclopenkune, cyclohexane, cyclohebutane, cyclooctane, cyclopropene,
Cyclobutene, cyclopentene, cyclohexene, / cloheptene, cyclooctene, limonene, tervirune,
7 Elandrene, silvestrene, tsene, carene, pifu:/, pornylene, kanghuen, fenchen, cyclobutanethiene, trinchrene, bisapolene, gingiberene, curcumene, humulene, casinosesquibenhen, serifene, caryophyllene, santarene, cedrene ,
Campholene, phylloclatene, podocarbrene, mylene, etc. are used. Examples of aromatic hydrocarbons include benzene, toluene, xylene, hemimelithene, pseudocumene, mesitylene, prenitene, indulene, durene, pentamethylbenzene, hexamethylbenzene,
Ethylbenzene, propylbenzene, cumene, styrene, biphenyl, terphenyl, diphenylmethane, triphenylmethane, dibenzyl, stilbene, indene,
Naphthalene, tetralin, anthracene, phenanthrene, etc. are used alone or in combination.
本発明における非晶質炭素膜中に含有される水素原子の
量は、用いる原料ガス、製造装置、成膜条件、並びにグ
ロー放電法という製法から必然的に定まるが、その量は
炭素原料と水素原料の総量に対して概ねｌＯ〜５Ｑａｔ
ｍ、％である。The amount of hydrogen atoms contained in the amorphous carbon film of the present invention is inevitably determined by the raw material gas used, the manufacturing equipment, the film forming conditions, and the manufacturing method called the glow discharge method. Approximately 1O~5Qat based on the total amount of raw materials
m,%.
本発明の非晶質炭素膜中には炭素、水素以外のへテロｇ
子、例えばフッ素、塩素、臭素あるいはヨウ素等のハロ
ゲン原子を含有させてもよい。The amorphous carbon film of the present invention contains heteroglycerides other than carbon and hydrogen.
It may also contain halogen atoms such as fluorine, chlorine, bromine or iodine.
ハロゲン原子の導入は、撥水性を向上させ、耐湿性を向
上させる。特に高湿環境下での複写画像流等に効果があ
り、その他に表面の滑り性を良くし、表面保護層の耐フ
ィルミング性を向上させることができる。係る効果はフ
ッ素原子を導入したときに特に大きい。Introduction of halogen atoms improves water repellency and moisture resistance. It is particularly effective in reducing the flow of copied images in high humidity environments, and can also improve the surface slipperiness and the filming resistance of the surface protective layer. This effect is particularly large when fluorine atoms are introduced.
ハロゲン原子を非晶質炭素膜に混入させるには、これら
の元素を含む適当なガス状化合物を炭化水素ガスと共に
、プラズマ状態にして成膜すればよい。もちろんそれら
の化合物における相状態は常温常圧において必ずしも気
相である必要はなく、加熱あるいは減圧等により溶融、
蒸発、昇華等を経て気化しうるものであれば、液相でも
固相でも使用可能である。In order to mix halogen atoms into an amorphous carbon film, a suitable gaseous compound containing these elements may be used together with a hydrocarbon gas in a plasma state to form the film. Of course, the phase state of these compounds does not necessarily have to be a gas phase at room temperature and pressure, but can be melted by heating or reduced pressure, etc.
As long as it can be vaporized through evaporation, sublimation, etc., either liquid phase or solid phase can be used.
少なくともハロゲン原子を含む分子としては、例えば、
フッ素、塩素、臭素、ヨウ素、フッ化水素、塩化水素、
臭化水素、ヨウ化水素、フッ化メチル、塩化メチル、臭
化メチル、ヨウ化メチル、７ツ化エチル、フッ化プロピ
ル、フッ化メチル、７ノ化アミル、フルオルベンゼン、
クロルベンゼン、フルオルスチレン、フルオロホルム、
クロロホルム、四フッ化炭素、フッ化ビニリデン、テト
ラフルオロエチレン、オクタフルオロプロパン等を用い
ることができる。Examples of molecules containing at least a halogen atom include:
Fluorine, chlorine, bromine, iodine, hydrogen fluoride, hydrogen chloride,
Hydrogen bromide, hydrogen iodide, methyl fluoride, methyl chloride, methyl bromide, methyl iodide, ethyl heptadate, propyl fluoride, methyl fluoride, amyl heptadide, fluorobenzene,
Chlorbenzene, fluorostyrene, fluoroform,
Chloroform, carbon tetrafluoride, vinylidene fluoride, tetrafluoroethylene, octafluoropropane, etc. can be used.
非晶質炭素膜中に含まれる上記ハロゲン原子の量は、プ
ラズマ反応に用いるハロゲン原子を含む分子の量を増減
することにより調整することができる。The amount of the halogen atoms contained in the amorphous carbon film can be adjusted by increasing or decreasing the amount of molecules containing halogen atoms used in the plasma reaction.
なお、上記へテロ原子の含有量はオージェ分析、元素分
析等の手段により知ることができる。The content of the above-mentioned heteroatoms can be determined by means such as Auger analysis and elemental analysis.
ここで、ハロゲン原子の添加量は０．１〜２５ａｔｍ、
％が適当である。２５ａｔｍ、％より多いと、摩擦帯電
電荷等が蓄積しやすい膜となり、０ 、 ］ ａｔｍ、
％より少ないとハロゲン原子を添加による効果を十分得
ることができない。Here, the amount of halogen atoms added is 0.1 to 25 atm,
% is appropriate. If the amount is more than 25 atm, the film will tend to accumulate triboelectric charges, etc., and 0, ] atm,
If the amount is less than %, the effect of adding halogen atoms cannot be sufficiently obtained.
本発明は、以上のようにしてプラズマ重合によって形成
された非晶質炭素膜をカルベン形成物質で処理する。In the present invention, the amorphous carbon film formed by plasma polymerization as described above is treated with a carbene-forming substance.
カルベン形成物質としては、下記構造式［１１；（式中
Ｘ１は水素またはハロゲン原子を表わす）であられされ
るケテン化合物また下記構造式［■］；／
Ｎ＝Ｎ＝Ｃ
＼
（式中Ｘ２は水素またはハロゲン原子を表わす）で表わ
されるジアゾ化合物を使用できる。Examples of carbene-forming substances include ketene compounds represented by the following structural formula [11; (wherein X1 represents hydrogen or a halogen atom) or the following structural formula [■]; / N=N=C \ (wherein X2 is It is possible to use diazo compounds represented by hydrogen or halogen atoms.
非晶質炭素膜のカルベン形成物質での処理は、非晶質炭
素膜の表面にカルベン形成物質がカルベン化して接触す
ればどのような方法でも良い。The treatment of the amorphous carbon film with the carbene-forming substance may be carried out by any method as long as the carbene-forming substance contacts the surface of the amorphous carbon film in a carbene-formed state.
非晶質炭素膜の表面が残留ラジカル、未結合手等が存在
する活性な状態であれば、カルベン形成物質を接触させ
るのみでも良く、（例えば、グロー放電によって非晶質
炭素膜を形成させ、そのまま真空を破らずにカルベン処
理する場合）非晶質炭素膜の表面が活性でない場合でも
、何らかの方法により該カルベン形成物質を活性化即ち
カルベン化して非晶質炭素膜に接触させれば良い。また
カルベン形成物質の蒸気に光をあて活性化して、あるい
は活性化させながら非晶質炭素膜に接触させることによ
り行なってもよい。例えば非晶質炭素膜を形成したグロ
ー放電分解装置を使用し、グロー放電分解重合に引き続
いてその反応槽中にカルベン形成物質の蒸気を送り込む
ことにより可能であり、所望により反応槽側壁に設けた
透明な窓から光を照射しながら連続的に行なうことがで
きる。If the surface of the amorphous carbon film is in an active state in which residual radicals, dangling bonds, etc. (When performing carbene treatment without breaking the vacuum) Even if the surface of the amorphous carbon film is not active, the carbene-forming substance may be activated, ie, carbene-ized, by some method and brought into contact with the amorphous carbon film. Alternatively, the vapor of the carbene-forming substance may be activated by exposing it to light, or may be brought into contact with the amorphous carbon film while being activated. For example, this can be done by using a glow discharge decomposition device on which an amorphous carbon film is formed, and feeding the vapor of a carbene-forming substance into the reaction tank following the glow discharge decomposition polymerization. This can be done continuously while shining light through a transparent window.
その他、カルベン形成物質が所望により活性化した状態
で非晶質炭素膜に接触させることができればいかなる方
法でもよく、例えば該カルベン形成物質を光励起、熱励
起、電子線励起、放射線動゛起等の方法により活性化さ
せることができるが、その際、プラズマ重合膜形成後カ
ルベン形成物質処理前の非晶質炭素膜は、水分、酸素等
で、本発明処理に使用するカルベン形成物質以外のガス
が付着・吸着あるいは反応しないように取扱うことが好
ましい。In addition, any method may be used as long as the carbene-forming substance can be brought into contact with the amorphous carbon film in an activated state as desired. For example, the carbene-forming substance may be activated by photoexcitation, thermal excitation, electron beam excitation, radiation activation, etc. However, in this case, the amorphous carbon film after forming the plasma polymerized film and before being treated with the carbene-forming substance is exposed to moisture, oxygen, and other gases other than the carbene-forming substance used in the treatment of the present invention. It is preferable to handle the material in a manner that prevents adhesion, adsorption, or reaction.
以上のようにして形成処理された非晶質炭素膜は、電荷
輸送層、電荷発生層、表面保護、下引き層または中間層
等の感光体構成部材等に使用可能である。またプラスチ
ックレンズ等の光学材の表面保護層としても使用可能で
、耐光性、耐環境性向上が期待でき、さらに静電摩擦帯
電制御部材としても、耐環境性の向上を期待できる。The amorphous carbon film formed as described above can be used as a component of a photoreceptor such as a charge transport layer, a charge generation layer, a surface protection layer, an undercoat layer, or an intermediate layer. It can also be used as a surface protective layer for optical materials such as plastic lenses, and can be expected to improve light resistance and environmental resistance.It can also be used as an electrostatic friction charge control member, and can be expected to improve environmental resistance.
第１図以下に、プラズマ重合非晶質炭素膜を感光体の構
成部材として使用した場合を説明する。A case in which a plasma-polymerized amorphous carbon film is used as a component of a photoreceptor will be described below with reference to FIG.
第１図中、（１）は基板、（２）は電荷発生層、（３）
は電荷輸送層を示す。In Figure 1, (1) is the substrate, (2) is the charge generation layer, (3)
indicates a charge transport layer.
基板は公知の種々のものを使用可能で、その上に設ける
電荷発生層も種々の無機系化合物あるいは有機系の化合
物から形成可能である。もちろんプラズマ重合膜から形
成してもよい。Various known substrates can be used, and the charge generation layer provided thereon can also be formed from various inorganic or organic compounds. Of course, it may be formed from a plasma polymerized film.
電荷輸送層（３）は、有機化合物をプラズマ重合するこ
とにより形成した非晶質炭素膜である。本発明は該電荷
輸送層をカルベン形成物質で処理する。有機化合物をプ
ラズマ重合して形成した非晶質炭素膜Ｉオ、前記したご
とく本来硬硬度で、耐摩耗性等に優れているが、本発明
の処理を処すことにより、さらに耐環境性に優れたもの
となり、感光体の初期特性を長期にわたり維持すること
ができる。The charge transport layer (3) is an amorphous carbon film formed by plasma polymerizing an organic compound. The present invention treats the charge transport layer with a carbene-forming substance. As mentioned above, the amorphous carbon film formed by plasma polymerization of an organic compound is inherently hard and has excellent wear resistance, but by applying the treatment of the present invention, it has even better environmental resistance. The initial characteristics of the photoreceptor can be maintained over a long period of time.
基板（１）上に電荷輸送層（３）および電荷発生層（１
シ）をこの順に設けた構成の感光体（第２図）において
も、プラズマ重合による非晶質炭素膜を電荷輸送層とし
て設けた場合はもちろん、電荷発生層（２）をプラズマ
重合により設けた場合にも本発明の処理は上記と同様の
効果がある。A charge transport layer (3) and a charge generation layer (1) are provided on the substrate (1).
In the photoreceptor (Fig. 2) with a structure in which (2) is provided in this order, as well as a case where an amorphous carbon film formed by plasma polymerization is formed as a charge transport layer, a charge generation layer (2) is formed by plasma polymerization. In this case, the treatment of the present invention has the same effect as above.
第３図および第４図の感光体は、それぞれ第１図および
第２図の構成の感光体にさらに表面保護層（４）を設け
たものである。本発明は、表面保護層（４）を非晶質炭
素膜で形成した感光体に適用したとき特に効果がある。The photoreceptors shown in FIGS. 3 and 4 are obtained by adding a surface protective layer (4) to the photoreceptors having the structures shown in FIGS. 1 and 2, respectively. The present invention is particularly effective when applied to a photoreceptor in which the surface protective layer (4) is formed of an amorphous carbon film.
電荷輸送Ｎ（３）あるいは電荷発生層（２）は必ずしも
プラズマ重合法により設け！１非晶質炭素膜である必要
はなく、従来から知られているものを使用することがで
きる。もちろん、グロー放電プラズマ重合法に設けた非
晶質炭素膜をそれらの層に適用し、本発明の処理を施し
てもよい。Charge transport N (3) or charge generation layer (2) is not necessarily provided by plasma polymerization! 1. It is not necessary to use an amorphous carbon film, and any conventionally known film can be used. Of course, amorphous carbon films prepared by glow discharge plasma polymerization may be applied to those layers and subjected to the treatment of the present invention.
表面保護層としての非晶質炭素膜には、水素以外のへテ
ロ原子、例えばフッ素、塩素、臭素あるいはヨウ素等ハ
ロゲン原子を含有する非晶質炭素膜とすることが好まし
い。そうすることにより、表面保護層の耐フィルミング
性を向上させることができ、係る効果はフッ素原子を導
入したとき特に大さい。また耐摩耗性等に有効である。The amorphous carbon film serving as the surface protective layer preferably contains a heteroatom other than hydrogen, such as a halogen atom such as fluorine, chlorine, bromine, or iodine. By doing so, the filming resistance of the surface protective layer can be improved, and this effect is particularly large when fluorine atoms are introduced. It is also effective in improving wear resistance.
非晶質炭素膜中のハロゲン原子の含有量が多くなりすぎ
ると、現像剤と表面保護層との摩擦帯電により、カブリ
が発生しやすくなるので注意を要する。If the content of halogen atoms in the amorphous carbon film becomes too large, fog is likely to occur due to frictional charging between the developer and the surface protective layer, so care must be taken.
第５図、第６図は非晶質炭素膜製造装置で容量結合型プ
ラズマＣＶＤ装置を示す。第５図は平行平板型プラズマ
ＣＶＤ装置、第６図は円筒型プラズマＣＶＤ装置を示す
。FIGS. 5 and 6 show a capacitively coupled plasma CVD apparatus which is an amorphous carbon film manufacturing apparatus. FIG. 5 shows a parallel plate type plasma CVD apparatus, and FIG. 6 shows a cylindrical type plasma CVD apparatus.
まず、第５図を用いて説明する。First, explanation will be given using FIG. 5.
第５図中、（７０１）〜（７０６）は常温において気相
状態にある原料化合物及びキャリアガスを密封した第１
乃至第６タンクで、各々のタンクは第１乃至第６Ｒ節弁
（７０７）〜（７１２）と第１乃至第６流量制御器（７
１３）〜（７１８）に接続されている。In FIG. 5, (701) to (706) are first tubes in which the raw material compound and carrier gas, which are in a gas phase at room temperature, are sealed.
Each tank has the first to sixth R control valves (707) to (712) and the first to sixth flow rate controllers (712).
13) to (718).
図中、（７１９）〜（７２１）は常温において液相また
は固相状態にある原料化合物を封入した第１乃至第３容
器で、各々の容器は気化のため第１乃至第３加熱器（７
２２）〜（７２４）により与熱可能であり、さらに各々
の容器は第７乃至第９調節弁（７２５）〜（７２７）と
第７乃至第９流量制御器（７２８）〜（７３０）に接続
されている。In the figure, (719) to (721) are first to third containers filled with raw material compounds that are in a liquid or solid phase at room temperature, and each container is connected to a first to third heater (721) for vaporization.
22) to (724), and each container is further connected to seventh to ninth control valves (725) to (727) and seventh to ninth flow rate controllers (728) to (730). has been done.
これらのガスは混合器（７３１）で混合された後、主管
（７３２）を介して反応室（７３３）に送り込まれる。These gases are mixed in a mixer (731) and then sent into a reaction chamber (733) via a main pipe (732).
途中の配管は、常温において液相または固相状態にあっ
た原料化合物が気化したガスが、途中で凝結しないよう
に、適宜配置された配管加熱器（７３４）により、与熱
可能とされている。The pipes along the way can be heated by appropriately placed pipe heaters (734) so that the gas, which is the vaporized raw material compound that is in a liquid or solid state at room temperature, does not condense on the way. .
反応室内には接地電極（７３５）と電力印加電極（７３
６）が対向して設置され、各々の電極は電極加熱器（７
３７）により与熱可能とされている。Inside the reaction chamber, there is a ground electrode (735) and a power application electrode (73).
6) are installed facing each other, and each electrode is connected to an electrode heater (7).
37) allows for heating.
電力印加電極には、高周波電力用整合器（７３８）を介
し°て高周波電源（７３９）、低周波電力用整合機（７
４０）を介して低周波電源（７４１）、ローパスフィル
タ（７４２）を介して直流電源（７４３）が接続されて
おり、接続選択スイッチ（７４４）により周波数の異な
る電力が印加可能とされている。The power application electrode is connected to a high frequency power source (739) and a low frequency power matching device (738) via a high frequency power matching device (738).
A low frequency power source (741) is connected through a low-frequency power source (741) and a DC power source (743) is connected through a low-pass filter (742), and power with different frequencies can be applied by a connection selection switch (744).
反応室内の圧力は圧力制御弁（７４５）により調整可能
であり、反応室内の減圧は排気系選択弁（７４６）を介
して、拡散ポンプ（７４７）、油回転ポンプ（７４８）
、或いは冷却除外装置（７４９）、メカニカルブースタ
ーポンプ（７５０）、油回転ポンプにより行われる。The pressure inside the reaction chamber can be adjusted by a pressure control valve (745), and the pressure inside the reaction chamber can be reduced through an exhaust system selection valve (746), a diffusion pump (747), and an oil rotary pump (748).
, or by a cooling exclusion device (749), mechanical booster pump (750), or oil rotary pump.
排ガスについては、さらに適当な除外装置（７５３）に
より安全無害化した後、大気中に排気される。The exhaust gas is further rendered safe and harmless by an appropriate exclusion device (753) before being exhausted into the atmosphere.
これら排気系配管に一ついても、常温において液相また
は同相状態にあった京料化合物が気化したガスが、途中
で凝結し、ないように、適宜配置された配管加熱器によ
り、与熱可能とされている。Even if one of these exhaust system piping is installed, heat can be provided by appropriately placed piping heaters to prevent the vaporized gas of the Kyoto compound, which is in liquid phase or the same phase at room temperature, from condensing on the way. has been done.
反応室も同様の理由から反応室加熱器（７５１）により
与熱可能とされ、内部に配された電極上に導電性基板（
７５２）が設置され乙。For the same reason, the reaction chamber can also be heated by a reaction chamber heater (751), and a conductive substrate (
752) has been installed.
これらの加熱器項は、使用さね、る原料ガスの性質に応
じて配するか否かを選択すれはよいが、特に、原料ガス
として常圧下での沸点が一５０°Ｃないし＋５０’Ｃの
何機化合物を用いた場合においては不要となる場合が臭
く、製・〜・装置の簡素化が可能となり好ましし・３
股に、訓点が一５０’Ｃよつ低い有機化合物を原料ガス
として用いた場合には、反応室（７３３）内部での微粉
状重合物の発生を防止するために、沸点が＋１５°Ｃよ
り高い有機化合物をぷ料ガスとして用いた場合には、各
種配管内での凝結防止のために、それぞれ上述の如き各
種加熱器を配することが望ましい。You can choose whether or not to install these heaters depending on the properties of the raw material gas to be used, but especially if the raw material gas has a boiling point of 150°C to +50'C under normal pressure. When organic compounds are used, they may become unnecessary, but it is preferable because it allows for the simplification of production equipment. In order to prevent the generation of fine powder polymer inside the reaction chamber (733), when an organic compound with a boiling point higher than +15°C is used as the fuel gas, In order to prevent condensation, it is desirable to provide various types of heaters as described above.
第５図において基板（７５２）は接地電極（７３５）に
固定して配されているが、電力印加電極（７３６）に固
定して配されてもよく、更に双方に配されていてもよい
。In FIG. 5, the substrate (752) is fixed to the ground electrode (735), but it may be fixed to the power application electrode (736), or may be fixed to both.
第６図に示した装置も基本的には第５図に示した装置と
同様であり、反応室（７３３）内の形態が基板（７５２
）が円筒形であることに応じて変更′！Ｊｔているもの
である。基板（７５２）は接地電極（７３５）を兼ね、
電力印加電極（７３６）および電極加熱器（７３７）共
に円筒形をなしている。また導電性基板（７５２）は、
外部より駆動モータ（７５４）を用いて、自転可能とな
っている。The apparatus shown in FIG. 6 is basically the same as the apparatus shown in FIG.
) is cylindrical, change accordingly′! This is what Jt is doing. The substrate (752) also serves as a ground electrode (735),
Both the power application electrode (736) and the electrode heater (737) have a cylindrical shape. In addition, the conductive substrate (752) is
It is rotatable using an external drive motor (754).
以上の構成において、反応室は、拡散ポンプ（７４７）
により予めＩＯ４乃至１ （’Ｊ −’Ｔｏｒｒ程度に
まで減圧し、真空度の確認と装置内部Ｃコ吸着］７たガ
スの脱着を行う。In the above configuration, the reaction chamber includes a diffusion pump (747)
The pressure is reduced to about IO4 to 1 ('J -' Torr, the degree of vacuum is confirmed, and the gas is adsorbed inside the apparatus), and the gas is desorbed.
同時に電極加熱器（７３７）により、電極（７３６）並
びに電極に固定して配された基板（７５２）を所定の温
度まで昇温する。At the same time, the electrode (736) and the substrate (752) fixedly disposed on the electrode are heated to a predetermined temperature by the electrode heater (737).
基板としては例えば導電性基板を用い、所望する非晶質
炭素膜に応じて、該基板を所定の温度に加熱する。For example, a conductive substrate is used as the substrate, and the substrate is heated to a predetermined temperature depending on the desired amorphous carbon film.
次いで、第１乃至第６タンク（７０１）〜（７０６）及
び第１乃至第３容器（７１９）〜（７２Ｄから原料ガス
を第１乃至第９流量制御器（７１３）〜（７１８）、（
７２８）〜（７３０）を用いて定流量化しながら反応室
（７３３）に導入し、圧力調節弁により反応室（７３３
）内を一定の減圧状態に保つ。Next, the raw material gas is transferred from the first to sixth tanks (701) to (706) and the first to third containers (719) to (72D) to the first to ninth flow rate controllers (713) to (718), (
728) to (730) to the reaction chamber (733) at a constant flow rate, and the pressure control valve to control the reaction chamber (733).
) to maintain a constant reduced pressure inside.
ガス流量が安定化した後、接続選択スイッチ（７４４）
により、たとえば高周波電源（７３９）を選択し、電力
印加電極（７３６）に高周波電力を投入する。After the gas flow rate has stabilized, press the connection selection switch (744)
For example, a high frequency power source (739) is selected, and high frequency power is applied to the power application electrode (736).
両電極間には放電が開始され、時間とともに基板上に固
相の有機プラズマ重合膜が形成される。A discharge is started between the two electrodes, and over time a solid phase organic plasma polymerized film is formed on the substrate.
本発明において非晶質炭素膜中に含まれる水素原子の量
は、成膜装置の形態並びに成膜時の茶件により変化し、
水素量が低くなる場合としては、例えば、基板温度が高
くする、圧力を低くする、原料炭化水素ガスの希釈率を
低くする、水素含有率の低い原料ガスを用いる、印加電
力を高くする、交番電界の周波数を低くする、交番電界
に重畳せしめた直流電界強度を高くする、等の場合が挙
げられる。In the present invention, the amount of hydrogen atoms contained in the amorphous carbon film varies depending on the form of the film forming apparatus and the conditions during film forming.
Examples of cases in which the amount of hydrogen decreases include raising the substrate temperature, lowering the pressure, lowering the dilution rate of the raw material hydrocarbon gas, using a raw material gas with a lower hydrogen content, increasing the applied power, and alternating Examples include lowering the frequency of the electric field and increasing the strength of the DC electric field superimposed on the alternating electric field.
非晶質炭素膜のカルベン形成物質による処理は、例えば
、以下のようにしておこなうことかできる。The treatment of the amorphous carbon film with a carbene-forming substance can be carried out, for example, as follows.
以上の工程で非晶質炭素膜を形成後、電力供給を停止し
、再び反応室（７３３）の内部のガスの脱気と装置内部
に付着あるいは吸着したガスの脱着を行ない、次いで、
第１〜第６タンク（７０１）〜（７０６）からカルベン
形成物質を第１〜第６流量制御器（７１３）〜（７１８
）を用いて定流量化しながら反応室（７３３）に導入し
、圧力調節弁により反応室（７３３）内を一定の減圧状
態に保つ。After forming the amorphous carbon film in the above steps, the power supply is stopped, and the gas inside the reaction chamber (733) is degassed and the gas attached or adsorbed inside the device is desorbed again.
The carbene forming substances are transferred from the first to sixth tanks (701) to (706) to the first to sixth flow rate controllers (713) to (718).
) is used to maintain a constant flow rate and introduced into the reaction chamber (733), and the inside of the reaction chamber (733) is maintained at a constant reduced pressure state by a pressure regulating valve.
ガス流量が安定化した後、反応室（７３３）の側壁に設
けた透明な窓（図示せず）から光、例えば短波長可視光
や紫外線を反応室内に照射し、カルベン形成物質を活性
化し、非晶質炭素膜に接触させる。After the gas flow rate is stabilized, light, such as short wavelength visible light or ultraviolet light, is irradiated into the reaction chamber through a transparent window (not shown) provided on the side wall of the reaction chamber (733) to activate the carbene-forming substance, Contact with an amorphous carbon film.
接触時間、温度、濃度等は、処理を施すべき非晶質炭素
膜の種類、カルベン形成物質の種類等に応じ適宜選定す
れはよい。The contact time, temperature, concentration, etc. may be appropriately selected depending on the type of amorphous carbon film to be treated, the type of carbene-forming substance, etc.
以下、実施例を挙げ本発明を説明する。The present invention will be explained below with reference to Examples.
衷寒倦
本実施例においては、導電性基板（１）上に、電荷発生
層（２）、電荷輸送層（３）およびオーバーコート層（
４）をこの順に設けた構成（第３図）の有機感光体を作
成し、該オーバーコート層（４）に本発明を適用した。In this example, a charge generation layer (2), a charge transport layer (3) and an overcoat layer (
An organic photoreceptor having a structure (FIG. 3) in which 4) were provided in this order was prepared, and the present invention was applied to the overcoat layer (4).
まず、円筒状アルミニウム基板（直径８０ｍｍＸ長さ３
３０ｍｍ）上に、以下に述べる感光層（電荷発生層十電
苛輸送層）を３種類下記したごとく作製しｔ二。First, a cylindrical aluminum substrate (diameter 80 mm x length 3
30 mm), three types of photosensitive layers (charge generation layer, charge transport layer) were prepared as described below.
有機系感光層Ａの作製
下記構造式（ｉ）で示されるジスアゾ化合物２重量部、
ポリエステル樹脂（東洋紡社製Ｖ−５００）１重量部、
メチルエチルケトン１００重量部をボールミルで、２４
時間分散した。この分散液を直径８０×長さ３３０ｍｍ
の円筒状アルミニウム基板上にディッピングにより乾燥
後の膜厚が３０００人となるように塗布し、電荷発生層
を形成した。Preparation of organic photosensitive layer A 2 parts by weight of a disazo compound represented by the following structural formula (i),
1 part by weight of polyester resin (V-500 manufactured by Toyobo Co., Ltd.),
In a ball mill, 100 parts by weight of methyl ethyl ketone was mixed with 24 parts by weight.
Spread out time. This dispersion liquid is 80 mm in diameter x 330 mm in length.
A charge generation layer was formed by dipping the mixture onto a cylindrical aluminum substrate so as to have a dry film thickness of 3000 nm.
次いで、この電荷発生層の上に、下記構造式（ｉ）で示
されるヒドラゾン化合物１０重量部、ポリカーボネイト
樹脂（帝人化成社製に−１３００）１０重量部をテトラ
ヒドロフラン８０重量部に溶解させた塗布液を乾燥後の
膜厚が２０μｍとなるように塗布、乾燥して電荷輸送層
を形成した。Next, on this charge generation layer, a coating solution containing 10 parts by weight of a hydrazone compound represented by the following structural formula (i) and 10 parts by weight of polycarbonate resin (manufactured by Teijin Kasei Co., Ltd. -1300) dissolved in 80 parts by weight of tetrahydrofuran was applied. was coated and dried to form a charge transport layer so that the film thickness after drying was 20 μm.
以上のようにして有機感光層Ａを得た。Organic photosensitive layer A was obtained as described above.
有機系感光層Ｂの作製
下記構造式（ｉｉ）に示されるジスアゾ化合物２重量部
、ポリエステル樹脂（東洋紡社製Ｖ−５００）ｌ 重ｊ
ｌ＆ メチルエチルケトン１００重量部をボールミルで
２４時間分散した。この分散液を直径８０×長さ３３０
ｍｍの円筒状アルミニウム基板上にディッピングにより
・乾燥後の膜厚が２５００人となるように塗布し、電荷
発生層を形成した。Preparation of organic photosensitive layer B 2 parts by weight of a disazo compound represented by the following structural formula (ii), polyester resin (V-500 manufactured by Toyobo Co., Ltd.)
100 parts by weight of methyl ethyl ketone were dispersed in a ball mill for 24 hours. This dispersion is 80mm in diameter x 330mm in length.
A charge generation layer was formed by coating on a cylindrical aluminum substrate with a thickness of 2,500 mm by dipping to a film thickness of 2,500 mm after drying.
次いで、この電荷発生層の上に、下記構造式（１ｖ）に
示されるスチリル系化合物１０重量部、ボリアリレート
樹脂（ユニチカ社製Ｕ−４０００）１０重量部をテトラ
ヒドロフラン８５重量部に溶解させた塗布液を乾燥後の
膜厚が２０μｍとなるように塗布、乾燥して電荷輸送層
を形成し、有機系感光層Ｂを得た。Next, on this charge generation layer, a solution of 10 parts by weight of a styryl compound represented by the following structural formula (1v) and 10 parts by weight of polyarylate resin (U-4000 manufactured by Unitika) dissolved in 85 parts by weight of tetrahydrofuran was applied. The liquid was coated so as to have a dry film thickness of 20 μm and dried to form a charge transport layer, thereby obtaining an organic photosensitive layer B.
有機系感光層Ｃの作製
下記構造式（Ｖ）に示されるジスアゾ化合物２重量部、
ポリエステル樹脂（東洋紡社製Ｖ−５００）１１Ｍ量８
、メチルエチルケトン１００重量部をボールミルで２４
時間分散した。この分散液を直径８０×長さ３３０ｍｍ
の円筒状アルミニウム基板上にディッピングにより乾燥
後の膜厚が３０００人となるように塗布し、電荷発生層
を形成した。Preparation of organic photosensitive layer C 2 parts by weight of a disazo compound represented by the following structural formula (V),
Polyester resin (V-500 manufactured by Toyobo Co., Ltd.) 11M amount 8
, 100 parts by weight of methyl ethyl ketone was milled in a ball mill to
Spread out time. This dispersion liquid is 80 mm in diameter x 330 mm in length.
A charge generation layer was formed by dipping the mixture onto a cylindrical aluminum substrate so as to have a dry film thickness of 3000 nm.
次いで、この電荷発生層の上に、下記構造式（ｖｉ）に
示されるスチリル系化合物１０重量部、メチルメタクリ
レート樹脂（三菱レーヨン社製ＢＲ−８５）１０重量部
をテトラヒドロフラン８０重量部に溶解させた塗布液を
乾燥後の膜厚が２０μｍとなるよう番こ塗布、乾燥１−
で電荷輸送層を形成し、有機系感光１Ｃを得た。Next, on this charge generation layer, 10 parts by weight of a styryl compound represented by the following structural formula (vi) and 10 parts by weight of methyl methacrylate resin (BR-85 manufactured by Mitsubishi Rayon Co., Ltd.) were dissolved in 80 parts by weight of tetrahydrofuran. Coat the coating solution so that the film thickness after drying is 20 μm, and dry 1-
A charge transport layer was formed using the above steps to obtain an organic photosensitive material 1C.
哀！霞七
上記で得らＪ−１だ有機系感光１に下記したごとく表面
保護層を作製（１、本発明による処理を施した。Sadness! Kasumi Seven A surface protective layer was prepared as described below on organic photosensitive material J-1 obtained above (1, the treatment according to the present invention was performed).
（表面保護層の作製）
第６図に示すグロー放′Ｉ！、分解装置においＣ１まず
反応室（７３３）の内部をＩ Ｏ−５Ｔｏｒｒ程度の高
真空にした後、第１、第２および第３調節弁（７０７）
、（７０８）および（７０９）を解放し、第１タン′７
（７０ｉ）よりテトラフルオロエチレン、第２タンク（
７０２）よリブテン、 第３タンクよりＨ２がスが出力
圧１．ｋｇ／ｃｍ”の下でマス７０−コントローラー（
７１３）、（７１４）および（７１５）内へ流入させた
。そして各マスフローコントローラーの目盛を調整して
、テトラフルオロエチレンｌ Ｏｓｃｃｍ、ブテン５
（Ｊ ｓｃｃｍ、 Ｈ２を１２０ｓｃｃｍとなるように
設定して反応室（７３３）内へ流入した。それぞれの流
量が安定した後に、反応室（７３３）の内圧がＱ−５Ｔ
ｏｒｒとなるよう調節し！こ。(Preparation of surface protective layer) Glow release 'I' shown in FIG. In the decomposition apparatus, first, the inside of the reaction chamber (733) is brought to a high vacuum of about IO-5 Torr, and then the first, second and third control valves (707)
, (708) and (709), and release the first tongue '7.
(70i) from tetrafluoroethylene, the second tank (
702) The output pressure of H2 from the third tank is 1. kg/cm” under mass 70-controller (
713), (714) and (715). Then, adjust the scale of each mass flow controller to obtain tetrafluoroethylene 1 Osccm, butene 5 Osccm,
(J sccm, H2 was set to 120 sccm and flowed into the reaction chamber (733). After each flow rate stabilized, the internal pressure of the reaction chamber (733) reached Q-5T.
Adjust so that it is orr! child.
一方、導電性円筒基板（７５２）、ｈに有磯系感光鳴Ａ
を設けた基板を用いて予め５０°Ｃに加熱しておき、各
ガス流量が安定し内圧が安定した状態で低周波電源（７
４１）を投入し、円筒型電極板（７３６）に１２Ｑｗａ
Ｌｔｓの電力（周波数２００ＫＨｚ）を印加して、約１
分４０秒間プラズマ重合を行ない、有機系感光層Ａ上に
厚さ約０．２２μｍの表面保護層を設けｌこ。On the other hand, on the conductive cylindrical substrate (752), Ariiso-based photosensitive ring A
Heat the substrate to 50°C in advance using a substrate equipped with
41) and put 12Qwa into the cylindrical electrode plate (736).
Approximately 1 by applying a power of Lts (frequency 200KHz)
Plasma polymerization was performed for 40 seconds to form a surface protective layer with a thickness of about 0.22 μm on the organic photosensitive layer A.
（表面ル理）
低周波電源（７４１）からの電力印加を一時停止し、反
応室内の内部登真空にした。(Surface Lubrication) The application of power from the low frequency power source (741) was temporarily stopped to create an internal vacuum inside the reaction chamber.
第４調節弁（７ｉ０）を解放し、第４タンク（７０４）
よ出力圧ゲージＩｋｇ／ｃｍ”の下でマス７０−コント
ローラー（７，１６）内へ流入させた。そしてマスフロ
ーコントローラーの目盛を調整して前記ケテン化合物の
流量を４０ ｓｅｃｍに設定し、反応室に流入させ、内
圧を０．６Ｔｏｒｒに調整し、主波長４８０ｎｍで半値
幅１１００ｎの光を図示しない窓から反応室（７３３）
内に照射し、その状態を３分間維持しｔ；。Release the fourth control valve (7i0) and release the fourth tank (704).
The ketene compound was allowed to flow into the mass 70-controller (7, 16) under an output pressure gauge of 1 kg/cm''. Then, the scale of the mass flow controller was adjusted to set the flow rate of the ketene compound to 40 sec, and the ketene compound was introduced into the reaction chamber. The internal pressure was adjusted to 0.6 Torr, and light with a main wavelength of 480 nm and a half-width of 1100 nm was emitted into the reaction chamber (733) through a window (not shown).
and maintain that state for 3 minutes.
なお、この時の基板温度は６０℃とした。Note that the substrate temperature at this time was 60°C.
得られた感光体の表面保護層中のフッ素原子の含有量は
表面保護層の全構成原子に対し２． ：３ ａｔｍｉｃ
％であった。The content of fluorine atoms in the surface protective layer of the obtained photoreceptor was 2. :3 atomic
%Met.
（評価）
得られた感光体を複写機（ＥＰ４７０Ｚ； ミノルタカ
メラ社製に搭載し高温高湿（３５°Ｃ１９０％）中に１
２時間放置した後の初期帯電電位（Ｖｏ）の減衰の程度
を評価し表１中に示した。(Evaluation) The obtained photoreceptor was mounted on a copying machine (EP470Z; manufactured by Minolta Camera Co., Ltd.) and placed in high temperature and high humidity (35°C, 190%) for 1 hour.
The degree of attenuation of the initial charging potential (Vo) after being left for 2 hours was evaluated and shown in Table 1.
表中 ○は実用上問題ない △は変化は認められるが実用上問題がない、 ×は実用上受は入れがたい ことを意味する。In the table, ○ indicates no practical problem. △ indicates a change is recognized but there is no practical problem. × is practically unacceptable It means that.
また、得られた感光体を−ａｏｏｖに初期帯電し白色光
を用いて一２００ｖに明減衰させるのに必要な光量を感
光体作製後と１年間大気環境下の室内に放置後のそれを
比較検討し、結果を表１に経時変化として示した。In addition, we compared the amount of light required to initially charge the obtained photoconductor to -aoov and attenuate the brightness to -200V using white light after fabricating the photoconductor and after leaving it indoors in an atmospheric environment for one year. The results are shown in Table 1 as changes over time.
表１中 Ｏは実用上問題ない △は変化は認められるが実用上問題が ない、 ×は実用上受は入れがたい ことを意味する。O in Table 1 has no practical problems. △ indicates a change is recognized but there is a practical problem. do not have, × is practically unacceptable It means that.
実施例２〜５
実施例１と同様にして、表１に示した感光層、表面ｉ頂
層作製条件およびその処理条件を適用し、実施例１と同
様に感光体を調整し評価した。Examples 2 to 5 In the same manner as in Example 1, photoreceptors were prepared and evaluated in the same manner as in Example 1 by applying the photosensitive layer, surface i-top layer manufacturing conditions, and processing conditions shown in Table 1.
結果を表１中に示した。The results are shown in Table 1.
比較例１〜３
表１に示した感光層、表面保護層作製条件を適用し、表
面処理を行なわなかった以外は実施例１と同様に感光体
を調製し評価した。Comparative Examples 1 to 3 Photoreceptors were prepared and evaluated in the same manner as in Example 1, except that the conditions for producing the photosensitive layer and surface protective layer shown in Table 1 were applied, and no surface treatment was performed.
結果を表１中に示した。The results are shown in Table 1.
実施例６
グロー放電分解装置（第５図）を用いて、導電性基板、
電荷輸送層、電荷発生層をこの順に設けた感光体を作製
した。Example 6 A conductive substrate,
A photoreceptor was prepared in which a charge transport layer and a charge generation layer were provided in this order.
（電荷輸送層形成工程ＸＣＴ Ｌ工程）：第５図に示す
グロー放電分解装置において、まず、反応装置（７３３
）の内部を１０− ’Ｔｏｒｒ程度の高真空にした後、
第１１及び第２調節弁（７０７、及び７０８）を解放し
、第１タンク（７０１）より水素ガス、及び第２タンク
（７０２）より１−３ブタジエンを各々出力圧１．０
Ｋｇ／ｃｍ”の下で第１１及び第２流量制御器（７１３
、及び７１４）内へ流入させた。そして各流量制御器の
目盛を調整して、水素ガスの流量を２００ｓｅｃｍ１１
−３ブタジエンガスの流量を６０ ｓｅｃｍとなるよう
に設定して、途中混合器（７３１）を介して、主管（７
３２）より反応室（７３３）内へ流入した。各々の流量
が安定した後に、反応室（７３３）内の圧力が０．５Ｔ
ｏｒｒとなるように圧力調節弁（７４５）を調整した。(Charge transport layer forming step XCT L step): In the glow discharge decomposition apparatus shown in FIG.
) After creating a high vacuum of about 10-' Torr inside the
The eleventh and second control valves (707 and 708) are opened, and hydrogen gas is supplied from the first tank (701) and 1-3 butadiene from the second tank (702) at an output pressure of 1.0.
11 and 2 flow controllers (713
, and 714). Then, adjust the scale of each flow rate controller to set the hydrogen gas flow rate to 200 sec11.
-3 The flow rate of butadiene gas was set to 60 sec, and the main pipe (7
32) into the reaction chamber (733). After each flow rate stabilizes, the pressure inside the reaction chamber (733) is 0.5T.
The pressure control valve (745) was adjusted so that the
一方、導電性基板（７５２）としては、縦５０×横５０
×厚３ｍｍのアルミニウム基板を用いて、予め１００°
Ｃに加熱しておき、ガス流量及び圧力が安定した状態で
、予め接続選択スイッチ（７４４）により接続しておい
た低周波電源（７４１）を投入し、電力印加電極（７３
６）に１ｏＯＷａｔｔの電力を周波数２００ＫＨｚの下
で印加して約３０分プラズマ重合反応を行ない、導電性
基板（７５２）上に厚さ１０μｍの非晶質炭素膜を電荷
輸送層として形成した。On the other hand, the conductive substrate (752) has a height of 50 x width of 50
× Using an aluminum substrate with a thickness of 3 mm,
C, and with the gas flow rate and pressure stable, turn on the low frequency power source (741) that was previously connected using the connection selection switch (744), and connect the power application electrode (73).
6), a plasma polymerization reaction was carried out for about 30 minutes by applying a power of 100 Watt at a frequency of 200 KHz to form a 10 μm thick amorphous carbon film as a charge transport layer on the conductive substrate (752).
成膜完了後は、電力印加を停止し、調節弁を閉じ、反応
室（７３３）内を充分に排気した。After the film formation was completed, power application was stopped, the control valve was closed, and the inside of the reaction chamber (733) was sufficiently evacuated.
以上のようにして得られた非晶質炭素膜につきＣＨＮ定
量分析を行なったところ、含有される水素原子の量は炭
素原子と水素原子の総量に対して４３ａｔｍｉｃ％であ
った。CHN quantitative analysis was performed on the amorphous carbon film obtained as described above, and the amount of hydrogen atoms contained was 43 atomic% with respect to the total amount of carbon atoms and hydrogen atoms.
（表面処理） 実施例１と同一の条件で表面処理を行なった。(surface treatment) Surface treatment was performed under the same conditions as in Example 1.
（電荷発生層形成工程）（ＣＧＬ工程）：第１調節弁（
７０７）、及び第６調節弁（７１２）を解放し、第１タ
ンク（７０１）から水素ガス、及び第６タンク（７０６
）からシランガスを、出力圧ＩＫｇ／ｃｍ２の下で第１
、第５、及び第６流量制御器（７１３，７１７及び７１
８）内へ流入させた。各流量制御器の目盛を調整して水
素ガスの流量を２１０ ｓｅｃｍ、及びシランガスの流
量を９Ｑｓｃｃｍに設定し、反応室（７３３）内に流入
させた。各々の流量が安定した後に、反応室（７３３）
内に圧力がｌ 、 ＯＴ （：＋ｒｒとなるように圧力
調節弁（７４５）を調整した。一方、非晶質炭素膜が形
成されている導電性基盤（７５２）は、１００°Ｃに加
熱しておき、ガス流量及び圧力が安定した状態で、高周
波電源（７３９）より周波数１３．５６ＭＨｚの下で電
力を印加し、グロー放電を発生させた。この放電を１５
分間行ない、厚さ；〕 ３μｍのａ−３ｉ：Ｈ電荷発生
層を形成しｔ：。(Charge generating layer forming process) (CGL process): First control valve (
707) and the sixth control valve (712) are released, and hydrogen gas is removed from the first tank (701) and the sixth tank (706).
) under an output pressure of IKg/cm2.
, fifth, and sixth flow rate controllers (713, 717, and 71
8) It was allowed to flow into the interior. The scales of each flow rate controller were adjusted to set the flow rate of hydrogen gas to 210 seconds and the flow rate of silane gas to 9Qsccm, which were then flowed into the reaction chamber (733). After each flow rate is stabilized, the reaction chamber (733)
The pressure regulating valve (745) was adjusted so that the pressure within the chamber was l, OT (:+rr).Meanwhile, the conductive substrate (752) on which the amorphous carbon film was formed was heated to 100°C. Then, with the gas flow rate and pressure stable, power was applied at a frequency of 13.56 MHz from a high frequency power source (739) to generate a glow discharge.This discharge was
A 3 μm thick a-3i:H charge generation layer was formed.
特性。Characteristic.
得られた感光体を常用のカールソンプロセスの中で用い
たところ最高帯電電位は一１０００Ｖ程度で有り、即ち
、全感光体膜厚が１０．３μｍであうことから１μｍ当
りの帯電能は約１００Ｖと極めて、高く、このことがら
充分な帯電性能を有するこ３−が確認された。また、暗
中にて一６００ｖから一５５０Ｖにまで暗減衰するのに
要した時間は約３５秒であり、このことから充分な電荷
保持性能を有することが確認された。また、−５００Ｖ
に初期帯電した後、白色光を用いて一１５０Ｖまで明減
衰させたところ必要とされた光量は約２゜１ルツクス・
秒であり、このことから充分な光感度性能を有すること
が確認された。また、本感光体を作製より６力月後に、
同様にして白色光感度測定を行なったところ、約２．３
ルツクス・秒で殆ど経時劣化を生じていないことが確認
された。When the obtained photoreceptor was used in a commonly used Carlson process, the highest charging potential was about -1,000 V. In other words, since the total photoreceptor film thickness was 10.3 μm, the charging ability was extremely high at about 100 V per 1 μm. , and this fact confirmed that it had sufficient charging performance. Further, the time required for dark decay from -600V to -550V in the dark was about 35 seconds, which confirmed that it had sufficient charge retention performance. Also, -500V
After initial charging, the brightness was attenuated to -150V using white light, and the amount of light required was approximately 2°1 Lux.
seconds, and from this, it was confirmed that the film had sufficient photosensitivity performance. Also, 6 months after the production of this photoreceptor,
When white light sensitivity was measured in the same way, the result was approximately 2.3.
It was confirmed that there was almost no deterioration over time in terms of Lux/second.
以上より、本例に示した本発明による感光体は、感光体
として優れた性能を安定に有するものである。また、こ
の感光体に対して常用のカールソンプロセスの中で、作
像して転写したところ、鮮明な画像が得られた。From the above, the photoreceptor according to the present invention shown in this example stably exhibits excellent performance as a photoreceptor. Further, when an image was formed and transferred to this photoreceptor using the commonly used Carlson process, a clear image was obtained.
一方、表面処理を施さなかった以外は本実施例と同様に
作製した感光体を６ケ月間大気環境下の室内に放置した
後、上記と同様に白色光感度を調べたところ７．３ルツ
クス・秒であった。このことより表面処理を施さない感
光体は、感度等の特性の経時変化が大きいことがわかる
。On the other hand, a photoreceptor manufactured in the same manner as in this example except that no surface treatment was applied was left indoors in an atmospheric environment for 6 months, and its white light sensitivity was examined in the same manner as above. It was seconds. From this, it can be seen that the photoreceptor without surface treatment has a large change in characteristics such as sensitivity over time.
発明の効果
本発明に従い処理されたプラズマで重合非晶質炭素膜は
、長期間の環境安定性に優れ、感光体製造工程中に、本
発明の処理を適用することにより、感光体特性の初期特
性が長期にわたって維持され、経時変化の少ない感光体
とすることができる。Effects of the Invention The plasma-polymerized amorphous carbon film treated according to the present invention has excellent long-term environmental stability, and by applying the treatment of the present invention during the photoreceptor manufacturing process, the initial characteristics of the photoreceptor can be improved. A photoreceptor whose properties are maintained over a long period of time and which undergoes little change over time can be obtained.
第１図〜第４図は感光体の構成例を示す図である。７
第５図および第６図は、７°〉ス′マ重合装置例の慨略
構、成を示す因である。
に）基板
（２）電荷発生層
（３）電荷輸送層
（・１）オーバーコート層
（７０１）〜（７０６）・・・タンク
（７０７）〜（７１２）及び（７２５）〜（７２７）・
・・調節弁（７１３）〜（７１８）及び（７２８）〜（
７３０）・・・ｉ 量制御器（マスフローコントローラ
ー）（７１９）〜（７２１）・・・容器（７２２）〜（
７２４）・・・温調器（７３１）・・・混合器 （
７３２）・・・主管（７３３）・・・反応室 （７
３４）・・・配管加熱器（７３５）・・・接地電極
（７３６）・・・電力印加電極（７３７）・・・電極加
熱器 （７３８）・・・高周波電力整合器（７３９）・
・・高周波電源
（７４０）・・・低周波電力用整合器
（７４１）・・低周ＥＡＫｉ （７４２）・・・ロー
パスフィルタ（７４３）・・・直流電源 （７４４）
・・・接続選択スイッチ（７４５）・・・圧力制御弁
（７４６）・・・排気系選択弁（７４７）・・拡散ポン
プ （７４８）・・・油回転ボ：／フ（７４９）・・・
冷却除外装置
（７５０）・・・メカニカルブースタポンプ（７５１）
・・・反応室加熱器 （７５２）・・・導電性基板（７
５３）・・・除外装置 （７５４）・・・駆動モータ
ー特許出願人 ミノルタカメラ株式会社FIGS. 1 to 4 are diagrams showing configuration examples of a photoreceptor. 7. FIGS. 5 and 6 show the general structure and structure of an example of a 7°>sma polymerization apparatus. 2) Substrate (2) Charge generation layer (3) Charge transport layer (・1) Overcoat layer (701) to (706)...tank (707) to (712) and (725) to (727)・
...Control valves (713) to (718) and (728) to (
730)...i Quantity controller (mass flow controller) (719) to (721)... Container (722) to (
724)...Temperature controller (731)...Mixer (
732)...Main pipe (733)...Reaction chamber (7
34)...Pipe heater (735)...Ground electrode
(736)...Power application electrode (737)...Electrode heater (738)...High frequency power matching device (739)...
...High frequency power supply (740) ...Low frequency power matching box (741) ...Low frequency EAKi (742) ...Low pass filter (743) ...DC power supply (744)
... Connection selection switch (745) ... Pressure control valve
(746)...Exhaust system selection valve (747)...Diffusion pump (748)...Oil rotary valve:/fu (749)...
Cooling exclusion device (750)...Mechanical booster pump (751)
... Reaction chamber heater (752) ... Conductive substrate (7
53)... Exclusion device (754)... Drive motor patent applicant Minolta Camera Co., Ltd.
Claims (1)
する感光体の製造方法において、該非晶質炭素膜をカル
ベン形成物質で処理する工程を含むことを特徴とする感
光体処理方法。1. A method for manufacturing a photoreceptor having an amorphous carbon film formed by a plasma polymerization method, the method comprising the step of treating the amorphous carbon film with a carbene-forming substance.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15289688A JPH023071A (en) | 1988-06-20 | 1988-06-20 | Process for treating photosensitive body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15289688A JPH023071A (en) | 1988-06-20 | 1988-06-20 | Process for treating photosensitive body |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH023071A true JPH023071A (en) | 1990-01-08 |
Family
ID=15550501
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP15289688A Pending JPH023071A (en) | 1988-06-20 | 1988-06-20 | Process for treating photosensitive body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH023071A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5218258A (en) * | 1990-09-04 | 1993-06-08 | Mitsubishi Jukogyo Kabushiki Kaisha | Ultrasonic motor and laser beam welding apparatus using the same |
-
1988
- 1988-06-20 JP JP15289688A patent/JPH023071A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5218258A (en) * | 1990-09-04 | 1993-06-08 | Mitsubishi Jukogyo Kabushiki Kaisha | Ultrasonic motor and laser beam welding apparatus using the same |
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