JPH0216913B2 - - Google Patents

Info

Publication number
JPH0216913B2
JPH0216913B2 JP12544282A JP12544282A JPH0216913B2 JP H0216913 B2 JPH0216913 B2 JP H0216913B2 JP 12544282 A JP12544282 A JP 12544282A JP 12544282 A JP12544282 A JP 12544282A JP H0216913 B2 JPH0216913 B2 JP H0216913B2
Authority
JP
Japan
Prior art keywords
evaporation
temperature
selenium
layer
tellurium
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.)
Expired
Application number
JP12544282A
Other languages
Japanese (ja)
Other versions
JPS5915942A (en
Inventor
Yukio Takano
Tatsuo Tanaka
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Fuji Electric Co Ltd
Original Assignee
Fuji Electric Co 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 Fuji Electric Co Ltd filed Critical Fuji Electric Co Ltd
Priority to JP12544282A priority Critical patent/JPS5915942A/en
Publication of JPS5915942A publication Critical patent/JPS5915942A/en
Publication of JPH0216913B2 publication Critical patent/JPH0216913B2/ja
Granted legal-status Critical Current

Links

Classifications

    • GPHYSICS
    • G03PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03GELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G5/00Recording members for original recording by exposure, e.g. to light, to heat, to electrons; Manufacture thereof; Selection of materials therefor
    • G03G5/02Charge-receiving layers
    • G03G5/04Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor
    • G03G5/08Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor characterised by the photoconductive material being inorganic
    • G03G5/082Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor characterised by the photoconductive material being inorganic and not being incorporated in a bonding material, e.g. vacuum deposited
    • G03G5/08207Selenium-based

Landscapes

  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Photoreceptors In Electrophotography (AREA)
  • Physical Vapour Deposition (AREA)

Description

【発明の詳細な説明】[Detailed description of the invention]

本発明は機能分離型のセレン・テルル感光体の
製造方法に関する。 電子写真用感光体として光導電材料としてセレ
ンを主体とした合金からなる感光層を導電性基板
上に形成したものが、複写機をはじめとして幅広
い分野で用いられている。最近この種の感光体に
おいて、特にその複写サイクルの繰返しによる特
性変動、すなわち疲労現象と呼ばれる残留電位の
上昇、帯電電位の低下を少なくすることおよびそ
の温度特性を改良する目的で光によりキヤリヤを
発生する層(電荷発生層またはCGL)と発生し
たキヤリア中の正孔が移動する層(電荷移動層ま
たはCTL)とを分離したいわゆる機能分離型の
多層感光体が一般的になつている。このような積
層された感光層を形成するには、CTLとして働
く第一層の蒸発が終了した後、真空蒸着槽の真空
状態を破壊し、さらに改めて第二層であるCGL
を蒸着する方法、あるいはCTLおよびCGLの両
層の蒸発源を蒸着槽内に並置し、各蒸発源の上部
にシヤツタ機構を備え、一方の蒸発源のシヤツタ
を閉じて他方の蒸発源による蒸着を行う方法が知
られている。しかしながら、これらの技術におい
ては、例えば前者の場合、蒸着時間の増加および
真空状態を破ることによる表面状態の悪化にに伴
う表面欠陥の発生の問題があり、後者の場合には
蒸着槽内に設けたシヤツタ機構へのセレンの付
着、再蒸発による感光層表面の欠陥の増加を防止
することは極めて困難である。 本発明の目的は、このような従来の多層蒸着の
欠点を除去し、表面欠陥が少なくかつサイクル特
性の極めてすぐれた感光体の製造方法を呈示する
ことにある。 この目的は、異なる組成比を有する複数のセレ
ン・テルル合金層を基体上にに積層するために、
一つの真空蒸着槽内に各組成比のセレン・テルル
合金の蒸発源を並置し、蒸着すべき層に対応する
蒸発源以外の蒸発源の温度を200〜300℃の範囲に
保ちながら順次蒸着を行うことによつて達成され
る。 以下図を引用し、本発明の実施例と比較例につ
いて説明する。第1図は実施例と比較例のための
装置を示し、円筒状真空槽1の軸方向に配置され
た円柱状支持軸2の上に感光体の導電性基体(基
板)3が取り付けられ、支持軸2の内部に設けら
れた温調系(ヒータ、水または液体温調)により
一定温度に保たれる。基体3の下方には第一層お
よび第二層用として二つの蒸発源4,5が位置す
る。蒸発源4,5の上に設けられたシヤツタ6,
7は比較例のためのもので本発明の実施例には使
用されない。 実施例 1 鏡面仕上げを施された直径120mm長さ288mmのア
ルミニウム製ドラムを硝酸溶液にて酸化処理を行
なつた後、第1図の装置内の支持軸2に設置し、
その温度を65℃に保持した。蒸発源4には、
Te5wt%のSe/Te合金を粒状化したものを1500
g、また、蒸発源5には13.5wt%のSe/Te合金
を500g入れ、まず蒸発源4の温度を340℃、蒸発
源5の温度を250℃に保持し、約40分第一層の蒸
着を行なつた後蒸発源4の温度を下げ250℃に保
持すると同時に蒸発体5の温度を350℃上昇せし
め約20分間蒸着を行なつた後に真空槽から取り出
してその電気特性及び外観、画像特性をチエツク
した。 実施例 2 実施例1ににおいて第一層のSe/Te合金の濃
度を2.0wt%にしたこと以外はすべて同様の条件
にて製造を行なつたものである。 比較例 実施例1と全く同様な材料を用いて蒸着を行つ
たものであるが、その蒸着制御方法としては、シ
ヤツタ6を開きシヤツタ7を閉じて蒸発源4の温
度を340℃として第一層の蒸着を終えた後、シヤ
ツタを開放して蒸発源5の温度を350℃として第
二層の蒸着を行つた。 以上の実施例および比較例により得られた感光
体の電気特性、外観および画像特性の結果を第1
表に示す。各例において試料数はn=50で画像テ
ストのみその内よりn=10について実施したもの
である。
The present invention relates to a method for manufacturing a functionally separated selenium/tellurium photoreceptor. 2. Description of the Related Art Photoreceptors for electrophotography, in which a photosensitive layer made of an alloy mainly composed of selenium as a photoconductive material is formed on a conductive substrate, are used in a wide range of fields including copying machines. Recently, in this type of photoreceptor, a carrier is generated by light for the purpose of reducing characteristic fluctuations caused by repeated copying cycles, that is, increases in residual potential and decreases in charged potential called fatigue phenomenon, and improving its temperature characteristics. A so-called functionally separated multilayer photoreceptor has become common, in which a layer (charge generation layer or CGL) for transporting holes is separated from a layer (charge transport layer or CTL) for transporting holes in generated carriers. To form such a laminated photosensitive layer, after the first layer serving as CTL has been evaporated, the vacuum state of the vacuum deposition tank is broken, and then the second layer, CGL, is evaporated.
Alternatively, the evaporation sources for both the CTL and CGL layers are arranged side by side in a deposition tank, and a shutter mechanism is installed above each evaporation source, so that the shutter of one evaporation source is closed and the evaporation by the other evaporation source is performed. There are known ways to do it. However, with these techniques, for example, in the former case, there is a problem of the generation of surface defects due to an increase in the deposition time and the deterioration of the surface condition due to breaking the vacuum state, and in the latter case, It is extremely difficult to prevent selenium from adhering to the shutter mechanism and increasing defects on the surface of the photosensitive layer due to re-evaporation. An object of the present invention is to eliminate such drawbacks of conventional multilayer deposition, and to present a method for manufacturing a photoreceptor with few surface defects and extremely excellent cycle characteristics. The purpose of this is to laminate multiple selenium-tellurium alloy layers with different composition ratios on a substrate.
Evaporation sources of selenium-tellurium alloys of various composition ratios are placed side by side in one vacuum evaporation tank, and the evaporation is performed sequentially while maintaining the temperature of the evaporation sources other than the evaporation source corresponding to the layer to be evaporated in the range of 200 to 300℃. It is achieved by doing. Examples and comparative examples of the present invention will be described below with reference to the drawings. FIG. 1 shows an apparatus for an example and a comparative example, in which a conductive base (substrate) 3 of a photoreceptor is mounted on a cylindrical support shaft 2 arranged in the axial direction of a cylindrical vacuum chamber 1. The temperature is maintained at a constant temperature by a temperature control system (heater, water or liquid temperature control) provided inside the support shaft 2. Two evaporation sources 4 and 5 are located below the substrate 3 for the first and second layers. a shutter 6 provided above the evaporation sources 4 and 5;
7 is for a comparative example and is not used in the examples of the present invention. Example 1 A mirror-finished aluminum drum with a diameter of 120 mm and a length of 288 mm was oxidized with a nitric acid solution, and then installed on the support shaft 2 in the apparatus shown in Figure 1.
The temperature was maintained at 65°C. Evaporation source 4 includes
1500 granulated Se/Te alloy with Te5wt%
g. Also, put 500g of 13.5wt% Se/Te alloy into the evaporation source 5, first keep the temperature of the evaporation source 4 at 340℃ and the temperature of the evaporation source 5 at 250℃, and heat the first layer for about 40 minutes. After the vapor deposition, the temperature of the evaporation source 4 was lowered and maintained at 250°C, and at the same time the temperature of the evaporator 5 was raised by 350°C, and after evaporation was performed for about 20 minutes, it was removed from the vacuum chamber and its electrical characteristics, appearance, and image were measured. I checked the characteristics. Example 2 Manufacturing was carried out under the same conditions as in Example 1 except that the concentration of the Se/Te alloy in the first layer was 2.0 wt%. Comparative Example Vapor deposition was carried out using the same material as in Example 1, but the vapor deposition was controlled by opening the shutter 6 and closing the shutter 7, setting the temperature of the evaporation source 4 to 340°C, and depositing the first layer. After completing the vapor deposition, the shutter was opened and the temperature of the evaporation source 5 was set at 350° C. to perform vapor deposition of the second layer. The results of the electrical characteristics, appearance, and image characteristics of the photoreceptor obtained in the above Examples and Comparative Examples are shown in the first example.
Shown in the table. In each example, the number of samples was n=50, and only the image test was performed on n=10 of them.

【表】 第1表においてVsは表面電位(V)の平均値、
E1/2は半減衰露光量(lx・sec)の平均値、画像
テストにおける評価方法は第2表の通りである。
[Table] In Table 1, Vs is the average value of surface potential (V),
E1/2 is the average value of half-attenuation exposure (lx·sec), and the evaluation method in the image test is as shown in Table 2.

【表】 第1表において、電気特性については平均値、
標準偏差σともにほぼ同等の結果を示している
が、外観および画像テストについては実施例と比
較例との間に明らかに有意差が認められる。この
ように本発明により表面欠陥を低減できる理由
は、蒸着すべき層に対応するもの以外の蒸発源の
温度をSe/Te合金の真空蒸気圧10-4に対応する
温度250℃に近い200℃以上に保持することによつ
てその蒸着源へのSe/Te合金の付着が防止され、
再蒸発による感光層表面への欠陥の生成が防止さ
れることにある。しかしこの保持温度が300℃を
超えると感光体への熱放射の影響により蒸着層の
結晶化等が生じ好ましくない。 上述のように本発明は、多層構造を有するセレ
ン・テルル感光体の蒸着工程において、当面の蒸
着源以外の蒸着源の温度を200〜300℃の範囲に保
持することによつて感光層表面に対する悪影響を
除くもので、途中で真空状態を破る必要なく、ま
たシヤツタなどの複雑な機構を持込む必要もな
く、蒸着源の温度制御だけによつて感光体の製造
歩留りの向上を図ることができる。勿論本発明は
2層構造に限定されることなく3層以上の多層構
造を有する感光体に対しても適用することが可能
であり、その効果は極めて大きい。
[Table] In Table 1, the electrical characteristics are average values,
Although the standard deviation σ shows almost the same results, there are clearly significant differences between the example and the comparative example in terms of appearance and image test. The reason why surface defects can be reduced by the present invention is that the temperature of the evaporation sources other than those corresponding to the layer to be evaporated is set to 200°C, which is close to 250°C, which corresponds to the vacuum vapor pressure of 10 -4 of the Se/Te alloy. By maintaining the temperature above, Se/Te alloy is prevented from adhering to the evaporation source.
The purpose is to prevent the formation of defects on the surface of the photosensitive layer due to re-evaporation. However, if this holding temperature exceeds 300° C., the deposited layer may crystallize due to the influence of thermal radiation on the photoreceptor, which is not preferable. As described above, in the vapor deposition process of a selenium/tellurium photoreceptor having a multilayer structure, the temperature of the vapor deposition sources other than the current vapor deposition source is maintained in the range of 200 to 300°C, thereby increasing the temperature of the photosensitive layer surface. It eliminates negative effects, there is no need to break the vacuum state during the process, there is no need to introduce a complicated mechanism such as a shutter, and it is possible to improve the production yield of photoreceptors simply by controlling the temperature of the evaporation source. . Of course, the present invention is not limited to a two-layer structure, but can also be applied to a photoreceptor having a multilayer structure of three or more layers, and its effects are extremely large.

【図面の簡単な説明】[Brief explanation of drawings]

第1図は本発明の実施例と比較例のための真空
蒸着装置の横断面図である。 1……真空槽、3……基体、4,5……蒸発
源。
FIG. 1 is a cross-sectional view of a vacuum evaporation apparatus for an example of the present invention and a comparative example. 1... Vacuum chamber, 3... Substrate, 4, 5... Evaporation source.

Claims (1)

【特許請求の範囲】[Claims] 1 異なる組成比を有する複数のセレン・テルル
合金層を基体上に積層するに際し、一つの真空蒸
着槽内に各組成比のセレン・テルル合金の蒸発源
を並置し、蒸着すべき層に対応する蒸発源以外の
蒸着源の温度を200〜300℃の範囲に保ちながら順
次蒸着を行うことを特徴とする電子写真用多層構
造セレン・テルル感光体の製造方法。
1. When laminating multiple selenium-tellurium alloy layers with different composition ratios on a substrate, evaporation sources for selenium-tellurium alloys with different composition ratios are placed side by side in one vacuum evaporation tank, and the evaporation sources correspond to the layers to be deposited. A method for manufacturing a multilayer selenium/tellurium photoreceptor for electrophotography, characterized in that deposition is carried out sequentially while maintaining the temperature of a deposition source other than the evaporation source within a range of 200 to 300°C.
JP12544282A 1982-07-19 1982-07-19 Manufacture of electrophotographic selenium-tellurium receptor having multilayered structure Granted JPS5915942A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP12544282A JPS5915942A (en) 1982-07-19 1982-07-19 Manufacture of electrophotographic selenium-tellurium receptor having multilayered structure

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP12544282A JPS5915942A (en) 1982-07-19 1982-07-19 Manufacture of electrophotographic selenium-tellurium receptor having multilayered structure

Publications (2)

Publication Number Publication Date
JPS5915942A JPS5915942A (en) 1984-01-27
JPH0216913B2 true JPH0216913B2 (en) 1990-04-18

Family

ID=14910186

Family Applications (1)

Application Number Title Priority Date Filing Date
JP12544282A Granted JPS5915942A (en) 1982-07-19 1982-07-19 Manufacture of electrophotographic selenium-tellurium receptor having multilayered structure

Country Status (1)

Country Link
JP (1) JPS5915942A (en)

Also Published As

Publication number Publication date
JPS5915942A (en) 1984-01-27

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