JPH029107B2 - - Google Patents

Info

Publication number
JPH029107B2
JPH029107B2 JP22306882A JP22306882A JPH029107B2 JP H029107 B2 JPH029107 B2 JP H029107B2 JP 22306882 A JP22306882 A JP 22306882A JP 22306882 A JP22306882 A JP 22306882A JP H029107 B2 JPH029107 B2 JP H029107B2
Authority
JP
Japan
Prior art keywords
boat
alloy
vapor deposition
evaporation
evaporation source
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
JP22306882A
Other languages
Japanese (ja)
Other versions
JPS59113180A (en
Inventor
Toshinao Ishisone
Hidenao Maeda
Kaneyuki Mantoku
Yoshinari Yoshimi
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 JP22306882A priority Critical patent/JPS59113180A/en
Publication of JPS59113180A publication Critical patent/JPS59113180A/en
Publication of JPH029107B2 publication Critical patent/JPH029107B2/ja
Granted legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation
    • C23C14/243Crucibles for source material

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Photoreceptors In Electrophotography (AREA)
  • Physical Vapour Deposition (AREA)

Description

【発明の詳細な説明】 〔産業上の利用分野〕 本発明は蒸着装置に係り、特に蒸着温度を異に
した2種の金属の薄膜を被蒸着物の表面に重ねて
形成できるようにした蒸着装置に関する。
[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a vapor deposition apparatus, and particularly to a vapor deposition apparatus that allows thin films of two types of metals at different vapor deposition temperatures to be formed on the surface of an object to be vaporized. Regarding equipment.

〔従来の技術〕 一般に真空蒸着は物体の表面に金属の薄膜を形
成する手段として広く知られており、金属または
その化合物を真空中でで加熱蒸発させることによ
り行われる。この真空蒸着方法は各方面で多用さ
れており、例えば電子写真用感光体の感光層とし
てセレンやセレンヒ素合金を導電性基板の上に形
成する際にも使用されている。
[Prior Art] Generally, vacuum evaporation is widely known as a means of forming a thin metal film on the surface of an object, and is performed by heating and evaporating a metal or its compound in a vacuum. This vacuum deposition method is widely used in various fields, and is also used, for example, when forming selenium or a selenium-arsenic alloy on a conductive substrate as a photosensitive layer of an electrophotographic photoreceptor.

セレンヒ素系感光体を使つた電子写真用感光体
においては、導電性基板に近い側をセレン含有量
の高い組成とし、その上に三セレン化二ヒ素
(As2Se3)の化学量論的組成を重ねて形成し、表
面にピンホールやスジ不良等が生じないようにし
ている。このような2層構造を有する光導電層を
真空蒸着法によつて形成する場合、従来は第1図
に示されるように、内部を真空とした蒸着容器1
内に被蒸着物としてのドラム状の基体2を配置
し、この基体2の下方に一層のセレン含有量の高
いセレンヒ系組成のAs2Se3組成の二層目蒸発源
4を配置している。そして、2つの蒸発源3,4
の加熱温度を個別的に制御できるようにするとと
もに、それぞれ異なる組成のセレンヒ素合金を適
切な蒸発温度にそれれ時間をずらして到達させる
ことによりそれぞれ対応するる一層目と二層目を
形成していた。
In an electrophotographic photoreceptor using a selenium-arsenic photoreceptor, the side closer to the conductive substrate has a composition with a high selenium content, and on top of that a stoichiometric composition of diarsenic triselenide (As 2 Se 3 ). The composition is layered to prevent pinholes, streak defects, etc. from occurring on the surface. When forming a photoconductive layer having such a two-layer structure by a vacuum evaporation method, conventionally, as shown in FIG.
A drum-shaped substrate 2 as an object to be evaporated is placed inside, and a second layer evaporation source 4 having a selenium-based composition of As 2 Se 3 with a high selenium content is placed below the substrate 2. . And two evaporation sources 3, 4
The heating temperature of the selenium arsenic alloys can be individually controlled, and the corresponding first and second layers can be formed by allowing the selenium arsenic alloys with different compositions to reach the appropriate evaporation temperature at different times. was.

〔発明が解決しようとする問題点〕[Problem that the invention seeks to solve]

しかしながら、このような従来の方法による時
には、加熱温度を異にした蒸発源が2つあつて、
それぞれ別個に温度制御されるため基体2の表面
に与える熱的変化の影響が大きく基体2の表面温
度がそれぞれの蒸着時にに一定になりにくく、こ
れが原因で膜厚にもバラツキを生じる傾向があつ
た。また、蒸発源が2つ、即ち熱源も別個に必要
になるのでそれだけ大きな熱量を消費することに
なり基体2のみならず蒸着容器1にも熱的影響を
及ぼし内壁にあらかじめ付着したセレンが剥離し
て塵となつて基体2の表面に付着することが多く
なり、これがピンホールの原因ともなつていた。
さらには熱エネルギーの使用効率も良くないとい
う問題があつた。
However, when using such conventional methods, there are two evaporation sources with different heating temperatures,
Since each temperature is controlled separately, the influence of thermal changes on the surface of the substrate 2 is large, making it difficult for the surface temperature of the substrate 2 to remain constant during each vapor deposition, which tends to cause variations in film thickness. Ta. In addition, since two evaporation sources, that is, separate heat sources, are required, a large amount of heat is consumed, which has a thermal effect not only on the substrate 2 but also on the deposition container 1, causing the selenium previously attached to the inner wall to peel off. This often turns into dust and adheres to the surface of the substrate 2, which also causes pinholes.
Furthermore, there was a problem that the efficiency of using thermal energy was not good.

そこで、本発明の目的は上述した従来技術が有
する欠点を解消し、蒸着膜の膜厚のバラツキが少
なくかつ表面にピンホールを生じない、特に電子
写真用感光層の形成に好適な蒸着装置を提供する
ことにある。
SUMMARY OF THE INVENTION Therefore, an object of the present invention is to solve the above-mentioned drawbacks of the prior art, and to provide a vapor deposition apparatus that is particularly suitable for forming a photosensitive layer for electrophotography, which has less variation in the thickness of a vapor-deposited film, and does not produce pinholes on the surface. It is about providing.

〔問題点を解決するための手段〕[Means for solving problems]

上記目的を達成するために本発明は、内部を真
空下に保持される蒸着容器内に被蒸着物を配置
し、この被蒸着物の下方に蒸発源を配置し、この
蒸発源は天壁の一部を開口した保温カバーと、こ
の保温カバー内に収容され、蒸気圧の異なる二種
の合金をそれぞれ収容するための第1および第2
のボートと、これらのボートのまわりに配置され
た加熱ヒータとを備える蒸着装置において、第1
および第2のボートのそれぞれは石英からなると
ともに、円筒の軸方向に平行な面で切り欠かれた
開口部を上部に備えた形状を有し、さらに上記第
1のボートと第2のボートとは保温カバーの開口
部直下に置かれたヒータの下方に第1ボートを上
側にして上下方向に重ね合わせるように配置され
ていることを特徴とするものである。
In order to achieve the above object, the present invention places an object to be evaporated in a vapor deposition container whose interior is kept under vacuum, and an evaporation source is arranged below the object to be evaporated. A heat insulating cover with a partially open area, and first and second insulating parts housed within the heat insulating cover for respectively accommodating two types of alloys having different vapor pressures.
In a vapor deposition apparatus comprising two boats and a heater arranged around these boats, a first
Each of the first boat and the second boat is made of quartz and has a shape with an opening cut out in a plane parallel to the axial direction of the cylinder, and the first boat and the second boat are each made of quartz. is characterized in that the heaters are placed below the heater placed directly under the opening of the heat insulating cover so as to be stacked vertically with the first boat on top.

以下、本発明による蒸着装置の実施例を第2図
および第3図を参照して説明する。
Embodiments of the vapor deposition apparatus according to the present invention will be described below with reference to FIGS. 2 and 3.

第2図において、符号11は内部を真空雰囲気
とした蒸着容器を示し、この蒸着容器11の内側
には被蒸着物としての基体12が配置されてい
る。この基体12は本実施例においては電子写真
用のドラムであつてその表面に光導電層を形成し
ようとするものである。この基体12の直下には
単一の蒸発源13が配置されている。この蒸発源
13は、第3図に拡大して示したように、保温カ
バー14を有し、保温カバー14の天壁の一部に
はスリツト15が開口してている。本実施例にお
いては保温カバー14はステンレス板を二重構成
することによつて構成されている。また、保温カ
バー14の内側には第1のボート16と第2のボ
ート17とが上下に積み重ねられるように配置さ
れている。これらのボート16,17は不透明な
石英で構成するのが好ましく断面がほぼ円の上方
の一部を切り欠いて開口部とした形態をなしてい
る。そして、第1のボート16内には一層目の蒸
発源として、例えばばSe濃度の高い75原子%Se
合金(以下A合金という)が所定量だけ装填され
ており、一方第2のボート17内には二層目の蒸
発源として三セレン化二ヒ素(As2Se3)の化学
量論的組成からなる合金(以下B合金という)が
所定量だけ装填されている。これらの合金につい
てはB合金よりA合金の蒸気圧の方が低いので、
同一真空条件下においては、A合金の方が早く蒸
着が始まることになる。さらに保温カバー14内
には上記第1のボート16と第2のボート17と
を包囲するように5個のヒータ装置18,18…
18が配置されている。これらのヒータ装置18
は赤外線ヒータを使用することが好ましくこれら
のヒータによつて保温カバー14内の温度を調節
することができる。また、上記第2のボート17
内には外部より温度を検出するためのセンサとし
て熱電対19が差し込まれている。
In FIG. 2, reference numeral 11 indicates a vapor deposition container whose interior is in a vacuum atmosphere, and a substrate 12 as an object to be vapor deposited is placed inside this vapor deposition container 11. In this embodiment, the substrate 12 is an electrophotographic drum on which a photoconductive layer is to be formed. A single evaporation source 13 is placed directly below this base 12 . As shown in an enlarged view in FIG. 3, this evaporation source 13 has a heat retaining cover 14, and a slit 15 is opened in a part of the top wall of the heat retaining cover 14. In this embodiment, the heat insulating cover 14 is constructed of double stainless steel plates. Furthermore, inside the heat retaining cover 14, a first boat 16 and a second boat 17 are arranged so as to be stacked vertically. These boats 16 and 17 are preferably made of opaque quartz and have a cross-section of a substantially circular shape with an upper portion cut out to form an opening. In the first boat 16, a first layer of evaporation source, for example, 75 atom% Se with a high Se concentration,
A predetermined amount of alloy (hereinafter referred to as alloy A) is loaded in the second boat 17, while a stoichiometric composition of diarsenic triselenide (As 2 Se 3 ) is loaded as a second layer evaporation source. (hereinafter referred to as B alloy) is loaded in a predetermined amount. Regarding these alloys, the vapor pressure of A alloy is lower than that of B alloy, so
Under the same vacuum conditions, the A alloy will start vapor deposition earlier. Further, inside the heat insulation cover 14, five heater devices 18, 18, . . . are provided so as to surround the first boat 16 and the second boat 17.
18 are arranged. These heater devices 18
It is preferable to use infrared heaters, and the temperature inside the heat retaining cover 14 can be adjusted by these heaters. In addition, the second boat 17
A thermocouple 19 is inserted inside as a sensor for detecting temperature from the outside.

〔作用〕[Effect]

このように構成された蒸着装置において、高真
空下でヒータ18を加熱すると、各蒸発源の温度
カーブ第4図に示したようになる。線1は第1ボ
ート16内のA合金の温度上昇カーブ、線2は第
2ボート17内のB合金の温度上昇カーブを示
す。線2のうち、蒸発源温度の平坦部は第3図の
熱電対19の先端部での温度であり、平坦に制御
されていることを示す。線1は熱電対19による
制御によれば、温度上昇速度が大きいことを示す
推測線である。この場合、第1のボート16内の
A合金は装填量が少なく、また開口部上のヒータ
18にB合金より近いので、温度上昇が大きく、
また蒸気圧の関係からB合金よりも時間的に早く
蒸発を開始し、装填した量が少ないためにB合金
の温度が蒸気圧に達するまでに蒸着が終了してし
まうように加熱が制御されている。したがつて、
第5図に示すとおり、基体12の表面にはまずA
合金による蒸着膜が一様に形成される。次いで、
B合金の蒸発が開始されA合金による薄膜の上に
B合金による薄膜が重ねて形成されるわけであ
る。
In the vapor deposition apparatus configured in this way, when the heater 18 is heated under high vacuum, the temperature curves of each evaporation source are as shown in FIG. 4. Line 1 shows the temperature rise curve of alloy A in the first boat 16, and line 2 shows the temperature rise curve of alloy B in the second boat 17. In line 2, the flat part of the evaporation source temperature is the temperature at the tip of the thermocouple 19 in FIG. 3, indicating that it is controlled flat. Line 1 is an estimated line indicating that the temperature rise rate is high according to the control by thermocouple 19. In this case, the A alloy in the first boat 16 has a small loading amount and is closer to the heater 18 above the opening than the B alloy, so the temperature rise is large.
Also, due to the vapor pressure, evaporation starts earlier than Alloy B, and since the amount loaded is small, the heating is controlled so that the vaporization ends before the temperature of Alloy B reaches the vapor pressure. There is. Therefore,
As shown in FIG. 5, the surface of the base 12 is first
A deposited film of the alloy is uniformly formed. Then,
Evaporation of the B alloy begins, and a thin film of the B alloy is formed on top of the thin film of the A alloy.

なお、上述した実施例においては第1のボート
16と第2のボート17とを不透明な石英ボート
で構成したが第1のボート16を透明の石英で構
成するととももに第2のボート17を不透明な石
英で構成するようにすると、さらにそれぞれの温
度上昇に差もたせ、異なる金属の二層蒸着を完全
なものとすることができる。
In the above embodiment, the first boat 16 and the second boat 17 were made of opaque quartz, but the first boat 16 was made of transparent quartz, and the second boat 17 was made of transparent quartz. If it is made of opaque quartz, it is possible to further differentiate the respective temperature rises and complete the two-layer vapor deposition of different metals.

また、上記実施例においてAs2Se3合金を使用
したが、これ以外に例えばSe−Te合金等につい
ても応用可能であることはもちろんである。
Further, although As 2 Se 3 alloy was used in the above embodiment, it is of course possible to use other alloys such as Se-Te alloy.

〔発明の効果〕 以上の説明から明らかなように、本発明によれ
ば蒸発源からの輻射熱を小さくして基本に付着し
た合金の再蒸発を防ぐようにしたために基体の表
面に形成される膜厚のバラツキをおさえることが
できる。また、熱エネルギーの使用効率が改善さ
れるので、蒸着容器の壁に付着したセレン等への
加熱時の熱影響が少なくなつてセレン合金が壁か
ら剥離して被蒸着物の表面に付着することも少な
くなり、その結果、ピンホール等を大幅に減少す
ることができる。
[Effects of the Invention] As is clear from the above explanation, according to the present invention, the radiant heat from the evaporation source is reduced to prevent re-evaporation of the alloy attached to the base, thereby reducing the film formed on the surface of the base. Variations in thickness can be suppressed. In addition, since the efficiency of using thermal energy is improved, the thermal effect on the selenium, etc. attached to the walls of the deposition container during heating is reduced, and the selenium alloy is less likely to peel off from the walls and adhere to the surface of the object to be deposited. As a result, pinholes and the like can be significantly reduced.

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

第1図は従来の蒸着装置を示した断面図、第2
図は本発明による蒸着装置の一実施例を示した断
面図、第3図は第2図の蒸発源を拡大して示した
断面図、第4図は蒸着時間と蒸発源温度との関係
を示した線図、第5図は蒸着膜内におけるセレン
の濃度分布を示した線図である。 11……蒸着容器、12……基体、13……蒸
発源、14……保温カバー、15……スリツト、
16……第1のボート、17……第2のボート、
18……ヒータ装置。
Figure 1 is a cross-sectional view of a conventional vapor deposition apparatus;
The figure is a sectional view showing an embodiment of the evaporation apparatus according to the present invention, FIG. 3 is an enlarged sectional view of the evaporation source shown in FIG. 2, and FIG. The diagram shown in FIG. 5 is a diagram showing the concentration distribution of selenium in the deposited film. 11... Vapor deposition container, 12... Substrate, 13... Evaporation source, 14... Heat insulation cover, 15... Slit,
16...first boat, 17...second boat,
18... Heater device.

Claims (1)

【特許請求の範囲】[Claims] 1 内部を真空下に保持される蒸着容器内に被蒸
着物を配置し、この被蒸着物の下方に蒸発源を配
置し、この蒸発源は天壁の一部を開口した保温カ
バーと、この保温カバー内に収容され、蒸気圧の
異なる二種の合金をそれぞれ収容するための第1
および第2のボートと、これらのボートのまわり
に配置された加熱ヒータとを備える蒸着装置にお
いて、第1および第2のボートのそれぞれは石英
からなるとともに、円筒の軸方向に平行な面で切
り欠かれた開口部を上部に備えた形状を有し、さ
らに上記第1のボートと第2のボートとは保温カ
バーのの開口部直下に置かれたヒータの下方に第
1ボートを上側にして上下方向に重ね合わせるよ
うに配置されていることを特徴とする装置。
1. An object to be evaporated is placed in a vapor deposition container whose interior is kept under vacuum, and an evaporation source is placed below the object. The first one is housed in the heat insulation cover and is used to accommodate two types of alloys having different vapor pressures.
and a second boat and a heater disposed around these boats, each of the first and second boats being made of quartz and cut in a plane parallel to the axial direction of the cylinder. The first boat and the second boat are arranged so that the first boat and the second boat are placed under a heater placed directly under the opening of the heat insulating cover, with the first boat on the top side. A device characterized in that it is arranged so as to overlap in the vertical direction.
JP22306882A 1982-12-21 1982-12-21 Vapor deposition device Granted JPS59113180A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP22306882A JPS59113180A (en) 1982-12-21 1982-12-21 Vapor deposition device

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP22306882A JPS59113180A (en) 1982-12-21 1982-12-21 Vapor deposition device

Publications (2)

Publication Number Publication Date
JPS59113180A JPS59113180A (en) 1984-06-29
JPH029107B2 true JPH029107B2 (en) 1990-02-28

Family

ID=16792323

Family Applications (1)

Application Number Title Priority Date Filing Date
JP22306882A Granted JPS59113180A (en) 1982-12-21 1982-12-21 Vapor deposition device

Country Status (1)

Country Link
JP (1) JPS59113180A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3008091U (en) * 1994-06-13 1995-03-07 オクス工業株式会社 High heel heel repair material

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN207398068U (en) * 2017-11-06 2018-05-22 北京汉能薄膜发电技术有限公司 A kind of device for preparing copper-indium-gallium-selenium compound

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3008091U (en) * 1994-06-13 1995-03-07 オクス工業株式会社 High heel heel repair material

Also Published As

Publication number Publication date
JPS59113180A (en) 1984-06-29

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