JPS62278565A - Selenium-tellurium material for electrophotographic sensitive body - Google Patents

Selenium-tellurium material for electrophotographic sensitive body

Info

Publication number
JPS62278565A
JPS62278565A JP12027186A JP12027186A JPS62278565A JP S62278565 A JPS62278565 A JP S62278565A JP 12027186 A JP12027186 A JP 12027186A JP 12027186 A JP12027186 A JP 12027186A JP S62278565 A JPS62278565 A JP S62278565A
Authority
JP
Japan
Prior art keywords
layer
sete
substrate
prescribed
alloy
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
Application number
JP12027186A
Other languages
Japanese (ja)
Inventor
Masahiro Sasaki
正廣 佐々木
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.)
Fujifilm Business Innovation Corp
Original Assignee
Fuji Xerox 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 Xerox Co Ltd filed Critical Fuji Xerox Co Ltd
Priority to JP12027186A priority Critical patent/JPS62278565A/en
Publication of JPS62278565A publication Critical patent/JPS62278565A/en
Pending 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
    • 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
    • G03G5/043Photoconductive layers characterised by having two or more layers or characterised by their composite structure
    • G03G5/0436Photoconductive layers characterised by having two or more layers or characterised by their composite structure combining organic and inorganic layers

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

Abstract

PURPOSE:To obtain an electrophotographic sensitive body having uniform characteristic value by regulating the atomic concn. of oxygen in an SeTe alloy as starting material to be evaporated to form an SeTe layer to prescribed ppm. CONSTITUTION:An Al pipe coated with an Al2O3 layer or a PET insulating layer, a laminate consisting of PET, Al, an electron injection preventive layer and a charge transferring layer of PVK or the like is used as a substrate. This substrate is placed in a vacuum deposition apparatus and an SeTe alloy having a prescribed O2 content is weighed and set as starting material to be evaporated. The apparatus is evacuated to a prescribed degree of vacuum and electric current is supplied to a resistance heating and evaporating source to evaporate the SeTe alloy. After a film is deposited to a prescribed thickness, the supply of electric current is stopped. Thus, a desired SeTe film is formed on the substrate.

Description

【発明の詳細な説明】 3、発明の詳細な説明 [産業上の利用分野] 本発明は電子写真に用いられる感光体用のセレンテルル
材料に関する。
Detailed Description of the Invention 3. Detailed Description of the Invention [Field of Industrial Application] The present invention relates to a selenite material for photoreceptors used in electrophotography.

[従来の技術] 電子写真感光体の高感度化の要請に伴ない、種々の増感
剤を混入させて目的を達成する努力か成されているが、
蒸着法によって感光層を形成する場合には構成成分の蒸
気圧、原子量等の違いにより、蒸発源組成か時間と共に
変化し、これに伴なって膜の組成も厚さ方向で変化して
しまうという不都合が有る。この不都合は、例えば感光
体の製品ばらつき増大による不良率の増大、感光体交換
時に複写条件を再設定する必要があること等、多大なコ
スト上昇を引き起す。このような不都合を改善するため
に、一方では多数の蒸発方法に関する提案が成されてい
るが、未だ決定的な改善には成り得ていない。
[Prior Art] With the demand for higher sensitivity of electrophotographic photoreceptors, efforts have been made to achieve the objective by mixing various sensitizers.
When forming a photosensitive layer by vapor deposition, the composition of the evaporation source changes over time due to differences in vapor pressure, atomic weight, etc. of the constituent components, and the composition of the film changes accordingly. There are inconveniences. This inconvenience, for example, increases the defective rate due to increased product variation in photoreceptors and requires resetting copying conditions when replacing photoreceptors, causing a significant increase in costs. In order to improve these inconveniences, many proposals regarding evaporation methods have been made, but no definitive improvement has yet been achieved.

[発明か解決しようとする問題点1 本発明は、通常の抵抗加熱型蒸発源を用い複雑な装置、
方法を用いることなく真空蒸着によりセレンテルル感光
層を形成する場合に於て、感光体としての特性値、詳し
くは受容電位、暗減衰、光感度等のばらつきを少なくし
、製品の不良率が低下するセレンテルル材料を提供する
ことを目的とするものである。
[Problem to be solved by the invention 1] The present invention uses a conventional resistance heating type evaporation source and a complicated device.
When a selenium tellurium photosensitive layer is formed by vacuum evaporation without using a method, variations in the characteristic values of a photoreceptor, specifically acceptance potential, dark decay, photosensitivity, etc., are reduced, and the defective rate of the product is reduced. The purpose of this invention is to provide a selenium tellurium material.

[問題点を解決するための手段] 本発明者は高感度化を達成するのに最も一般的なセレン
テルル(SeTe)材料を感光層とする電子写真感光体
に関し、蒸着技術とは別に材料について鋭意研究の結果
、感光層としてのSeTe合金に含有される醇索溌度か
める値より大きいときに上記不都合を引き起しているこ
とを明確にした。すなわち、酸素濃度の変化に伴ない、
蒸着膜の厚さ方向のSe/Te組成が著しく変化し、延
いては感光体の製品ばらつきに著しい変化を与えている
ことを見出し、この知見に基づいて本発明を完成した。
[Means for Solving the Problems] The present inventors have made extensive efforts regarding materials in addition to vapor deposition techniques regarding electrophotographic photoreceptors whose photosensitive layer is selenium telluride (SeTe), which is the most common material used to achieve high sensitivity. As a result of research, it has been clarified that the above-mentioned disadvantages occur when the solubilization strength contained in the SeTe alloy used as the photosensitive layer is larger than the value. In other words, as the oxygen concentration changes,
It was discovered that the Se/Te composition in the thickness direction of the deposited film changes significantly, which in turn causes a significant change in the product variation of photoreceptors, and based on this knowledge, the present invention was completed.

すなわち、本発明は導電性を有する支持体上に感光層と
して5eTe層を持つ電子写真感光体に関し、5eTe
層を形成する蒸発前の母材料で必る 3eTe合金に含
有される酸素原子濃度を1001)13m以下、望まし
くは1oppm以下にしたことを特徴とする。
That is, the present invention relates to an electrophotographic photoreceptor having a 5eTe layer as a photosensitive layer on a conductive support.
It is characterized in that the concentration of oxygen atoms contained in the 3eTe alloy, which is necessary in the base material before evaporation to form the layer, is 1001)13m or less, preferably 1 oppm or less.

本発明の詳細を以下に記す。The details of the invention are described below.

電子写真感光体に用いられる導電性を有する支持体とし
ては、例えばA I、Mo、Au、in、Nb、Ta、
N i、v、Ti、Pt、Pd、 Cr、pb等の金属
、又はこれら合金等の導電性支持体であり絶縁性支持体
の場合には必要に応じて、例えば、PET、ポリイミド
フィルムの場合にはフィルム上に上記導電性材料の薄膜
が形成されたものを用いる。薄膜化される導電性材料と
しては他にも■n203、SnO2、CuI等が挙げら
れる。
Examples of conductive supports used in electrophotographic photoreceptors include AI, Mo, Au, in, Nb, Ta,
A conductive support made of a metal such as Ni, V, Ti, Pt, Pd, Cr, PB, or an alloy thereof, and in the case of an insulating support, as necessary, for example, in the case of PET or polyimide film. A film in which a thin film of the above conductive material is formed on the film is used. Other examples of the conductive material to be made into a thin film include n203, SnO2, CuI, and the like.

また支持体の形状については、円筒状、平板状、シート
状、スクリーン状等何れの場合でもよい。
The shape of the support may be cylindrical, flat, sheet, screen, or the like.

上記支持体上に、電子写真感光体の構成として、静電潜
像形成プロセス、又は使用材料の特性に応じて電荷注入
層、電荷注入阻止層、電荷輸送層、絶縁層、表面層、保
護層等を静電潜像が形成される様に機能的に積層する。
On the above support, as a structure of the electrophotographic photoreceptor, a charge injection layer, a charge injection blocking layer, a charge transport layer, an insulating layer, a surface layer, a protective layer are formed according to the electrostatic latent image forming process or the characteristics of the materials used. etc. are laminated functionally so that an electrostatic latent image is formed.

電子写真感光体の構成としては前記した層以外に感光性
の層(以下電荷発生層と略す。)を必要とする。
The structure of the electrophotographic photoreceptor requires a photosensitive layer (hereinafter abbreviated as charge generation layer) in addition to the above-mentioned layers.

本発明はこの電荷発生層の材料に関するものでおる。基
板としては、目的とする機能が得られる層構成となるも
のを使用する。例えば、Al2O3処理を施されたAI
パイプ、PET絶縁層、PET上にNiCr、AIの如
き導電性膜を施したもの、更にはPET−A I−電子
注入阻止層−PVK等の電荷輸送層を積層したもの等が
用いられる。
The present invention relates to the material of this charge generation layer. The substrate used has a layered structure that provides the desired function. For example, AI treated with Al2O3
A pipe, a PET insulating layer, a conductive film such as NiCr or AI formed on PET, and a stacked charge transport layer such as PET-A I-electron injection blocking layer-PVK are used.

これらの基板を、真空蒸着装置槽内に設置し、蒸発源と
して本発明の意図する02含量となるように5eTeの
原料を秤量しセットづる。
These substrates are placed in a vacuum evaporation equipment tank, and 5eTe raw material is weighed and set so as to have the 02 content as intended by the present invention as an evaporation source.

すなわら高純度のSeおよびTeと02含量か所望の値
となるようにTeO2を秤量して、セットし、槽内を排
気する。
That is, high-purity Se and Te and TeO2 are weighed and set so as to have the desired content, and the inside of the tank is evacuated.

所定の真空度、例えば1X10−5Torrに排気した
後、抵抗加熱蒸発源に通電し、5eTe原料を蒸発させ
る。所定の膜厚を得た後、通電を停止し基板上に所望の
5eTe膜が形成される。
After evacuation to a predetermined degree of vacuum, for example 1×10 −5 Torr, electricity is applied to the resistance heating evaporation source to evaporate the 5eTe raw material. After obtaining a predetermined film thickness, the current supply is stopped and a desired 5eTe film is formed on the substrate.

なお、本発明の5eTe材料の製造方法は上記の例に限
定されず、例えば系内を徹底的に非酸化性雰囲気として
、或いは積極的に還元性雰囲気を実現して(qられる5
eTe合金であってもよく、製法による制約を受けるも
のではない。
Note that the method for producing 5eTe material of the present invention is not limited to the above example, and for example, the system may be thoroughly created with a non-oxidizing atmosphere or a reducing atmosphere may be actively created (q.
It may be an eTe alloy, and is not limited by the manufacturing method.

所望の5eTe合金材料層が形成された後、更に静電潜
像を形成するに必要な他の層を積層するか、乃至は積層
せずに電子写真感光体が作られる。
After the desired 5eTe alloy material layer is formed, an electrophotographic photoreceptor is fabricated with or without laminating other layers necessary to form an electrostatic latent image.

:!実施例1 以下本発明の5eTe材料に関して図面を参照しながら
実施例に基づいて説明する。
:! Example 1 The 5eTe material of the present invention will be described below based on an example with reference to the drawings.

実施例1 99、999%seと99.9999%Teをパイレッ
クスアンプル内に真空封入した後、撮盪炉を用い、55
0’Cで2時間混合した。その後急令し、Te40重量
%の5eTe合金を得た。
Example 1 After vacuum sealing 99,999% se and 99.9999% Te in a Pyrex ampoule, 55%
Mixed for 2 hours at 0'C. Thereafter, a 5eTe alloy containing 40% by weight of Te was obtained.

この合金を細粉砕し、加圧成型機にて8φ、厚み2#の
錠剤状の5eTe材料を作った。第1図に示す真空装置
1でAl2O3処理を施したA1パイプ2を基板とし、
基板温度75°Cに昇温した。
This alloy was finely pulverized and a tablet-shaped 5eTe material having an diameter of 8 and a thickness of 2 # was produced using a pressure molding machine. The substrate is an A1 pipe 2 which has been subjected to Al2O3 treatment in the vacuum device 1 shown in FIG.
The substrate temperature was raised to 75°C.

抵抗加熱蒸発源3に基板に成膜される膜の厚みが50μ
になる様に秤量されたSeを充填した。抵抗加熱蒸発源
4に、上述した3e’l’−e材料を、基板に成膜され
る膜の厚みが1μになる様に秤量しセットした。
The thickness of the film formed on the substrate in the resistance heating evaporation source 3 is 50μ.
It was filled with Se weighed so that The above-mentioned 3e'l'-e material was weighed and set in the resistance heating evaporation source 4 so that the thickness of the film formed on the substrate was 1 μm.

、槽内を排気し、1 x 1’Q−5Torrに至った
後、蒸発源3に通電し、図示していない制御系(熱電対
)により350’Cまで昇温し、20分間保持し、Se
を基板上に50μ厚に成膜した。その後、同様に蒸発源
4に通電し、図示していない制御系(熱電対)により4
50’Cまで昇温し、3分間保持し5eTeを基板仮に
1μ厚に成膜した。その後通電を停止し、槽内を大気圧
に戻し、第2図に示す様な構成を有する電子写真感光板
を得た。尚、同じ操作を更に5回繰り返し6個のサンプ
ルを得た。
After evacuating the tank and reaching 1 x 1'Q-5 Torr, the evaporation source 3 was energized, and the temperature was raised to 350'C by a control system (thermocouple) not shown, and held for 20 minutes. Se
was formed on a substrate to a thickness of 50 μm. After that, the evaporation source 4 is energized in the same way, and a control system (thermocouple) not shown is used to energize the evaporation source 4.
The temperature was raised to 50'C and maintained for 3 minutes to form a film of 5eTe to a thickness of 1 μm on the substrate. Thereafter, the electricity supply was stopped and the pressure inside the tank was returned to atmospheric pressure, thereby obtaining an electrophotographic photosensitive plate having the structure shown in FIG. 2. The same operation was repeated five more times to obtain six samples.

実施例2 99、999%Seと99.9999%TeとTeO2
を酸素原子比か10ppmになる様に秤量し、パイレッ
クスアンプル内に真空封入した後、振盪炉を用い、55
0°Cにて2時間混合した。その後急令し、Te40重
量%で、含有酸素原子比10pDmの5eTe合金を得
た。この材料を用いた他は実施例1と全く同じ手法にて
電子写真感光板を(qた。
Example 2 99.999% Se, 99.9999% Te and TeO2
was weighed so that the oxygen atomic ratio was 10 ppm, vacuum-sealed in a Pyrex ampoule, and then heated in a shaking oven.
Mixed for 2 hours at 0°C. Thereafter, a 5eTe alloy containing 40% by weight of Te and an atomic ratio of oxygen of 10 pDm was obtained. An electrophotographic photosensitive plate was prepared in exactly the same manner as in Example 1 except that this material was used.

実施例3 99、999%Seと99.9999%TeとTeO2
を酸素原子比が1100ppになる様に秤量し、パイレ
ックスアンプル内に真空封入した後、振盪炉を用い、5
50’Cにて2時間混合した。その後急令し、Te40
重量%、含有酸素原子比1100ppの5eTe合金を
1qだ。この材料を用いた他は実施例1と全く同じ手法
にて電子写真感光板を得た。
Example 3 99.999% Se, 99.9999% Te and TeO2
was weighed so that the oxygen atomic ratio was 1100 pp, vacuum sealed in a Pyrex ampoule, and then heated in a shaking oven for 5
Mixed for 2 hours at 50'C. After that, an urgent order was made and Te40
1q of 5eTe alloy with weight% and oxygen atomic ratio of 1100pp. An electrophotographic photosensitive plate was obtained in exactly the same manner as in Example 1 except that this material was used.

実施例4 実施例2.3と同様にして含有酸素原子比1.000p
pmの5eTe合金(Te40@量%)を得た。この材
料を用いた他は実施例1と全く同じ手法にて電子写真感
光板を1qだ。
Example 4 Same as Example 2.3, containing oxygen atomic ratio 1.000p
A 5eTe alloy (Te40@mass%) of pm was obtained. An electrophotographic photosensitive plate of 1 q was prepared in exactly the same manner as in Example 1 except that this material was used.

実施例5 実施例4と同様にしてTe40重量%で、含有酸素原子
比10. OOOppmの5eTe合金を得た。この材
料を用いた他は実施例1と全く同じ手法にて電子写真感
光板を(qた。
Example 5 In the same manner as in Example 4, Te was 40% by weight and the oxygen atomic ratio was 10. A 5eTe alloy of OOOppm was obtained. An electrophotographic photosensitive plate was prepared in exactly the same manner as in Example 1 except that this material was used.

以上、実施例1〜5に記述した電子写真感光板の電気特
性の測定を行ない、第3図(a)に示す様な暗部電位、
第3図(b)に示す光感度を(qた。尚、図中、黒丸は
6個の電子写真感光板サンプルの平均値を示す。
As described above, the electrical characteristics of the electrophotographic photosensitive plates described in Examples 1 to 5 were measured, and the dark area potential as shown in FIG.
The photosensitivity shown in FIG. 3(b) was (q). In the figure, the black circles indicate the average value of six electrophotographic photosensitive plate samples.

第3図(a)及び(b)から明らかな様に、含有酸素原
子比濃度が100 ppmを超えると暗電位の帯電性が
悪く、ばらつきも多くなり、中には全く帯電しないサン
プルも発生した。また光感度に関しても1oopp…を
超えると著しくばらつく様になった。
As is clear from Figures 3 (a) and (b), when the atomic concentration of oxygen exceeds 100 ppm, the charging properties of the dark potential become poor and there are many variations, and some samples were not charged at all. . In addition, the photosensitivity began to vary significantly when it exceeded 1oopp.

一方10.000ppmの酸素含有5eTeは暗部電位
、光感度共に比較的安定した特性を示したが長波長に於
ける光感度か低下してしまうという不都合が発生した。
On the other hand, 5eTe containing 10.000 ppm of oxygen showed comparatively stable characteristics in terms of dark potential and photosensitivity, but had the disadvantage that photosensitivity at long wavelengths decreased.

[発明の効果] 本発明は電子写真感光体用セレンテルル材料として、酸
素原子9度1100pp以下の材料を提供したもので必
り、本発明の材料を用い、蒸着法によって感光層を形成
することにより容易に特性値にばらつきの少ない電子写
真感光体を製造することかできる。
[Effects of the Invention] The present invention provides a selenium tellurium material for electrophotographic photoreceptors, which has an oxygen atom of 9 degrees and 1100 pp or less. Electrophotographic photoreceptors with less variation in characteristic values can be easily manufactured.

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

第1図は真空蒸着装置の概要図、 第2図は電子写真感光体の一例の断面図、第3図(a)
は含有酸素原子比と暗電位の関係を示す図、 第3図(b)は含有酸素原子比と80Qnmに於ける光
感度の関係を示す図である。 図中符号: 1・・・真空蒸着装置; 2・・・基板; 3,4・・
・蒸発源。 第1図 第2図 第3図(、l) 0  10   TOO1α℃ 1顛 @M酸p+謳ヒ ppm 含有南艷享J敢号寸ヒ ppm
Figure 1 is a schematic diagram of a vacuum evaporation device, Figure 2 is a sectional view of an example of an electrophotographic photoreceptor, and Figure 3 (a).
FIG. 3B is a diagram showing the relationship between the atomic ratio of oxygen contained and the dark potential, and FIG. 3(b) is a diagram showing the relationship between the atomic ratio of oxygen contained and photosensitivity at 80 Q nm. Symbols in the figure: 1... Vacuum evaporation device; 2... Substrate; 3, 4...
・Evaporation source. Figure 1 Figure 2 Figure 3 (,l) 0 10 TOO1α℃ 1@M acid p+single ppm Containing Nansho KyoJGiangosunhi ppm

Claims (1)

【特許請求の範囲】[Claims] 導電性支持体上に蒸着によって形成する電子写真感光体
の感光層用のセレンテルル材料であって、酸素原子濃度
が100ppm以下であることを特徴とするセレンテル
ル材料。
A selenite material for a photosensitive layer of an electrophotographic photoreceptor formed on a conductive support by vapor deposition, the selenite material having an oxygen atom concentration of 100 ppm or less.
JP12027186A 1986-05-27 1986-05-27 Selenium-tellurium material for electrophotographic sensitive body Pending JPS62278565A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP12027186A JPS62278565A (en) 1986-05-27 1986-05-27 Selenium-tellurium material for electrophotographic sensitive body

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP12027186A JPS62278565A (en) 1986-05-27 1986-05-27 Selenium-tellurium material for electrophotographic sensitive body

Publications (1)

Publication Number Publication Date
JPS62278565A true JPS62278565A (en) 1987-12-03

Family

ID=14782091

Family Applications (1)

Application Number Title Priority Date Filing Date
JP12027186A Pending JPS62278565A (en) 1986-05-27 1986-05-27 Selenium-tellurium material for electrophotographic sensitive body

Country Status (1)

Country Link
JP (1) JPS62278565A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008227036A (en) * 2007-03-12 2008-09-25 Fujifilm Corp Radiation plane detector

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59166961A (en) * 1983-03-12 1984-09-20 Ricoh Co Ltd Electrophotographic sensitive body
JPS59223436A (en) * 1983-06-03 1984-12-15 Fuji Xerox Co Ltd Photosensitive body of selenium-tellurium alloy

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59166961A (en) * 1983-03-12 1984-09-20 Ricoh Co Ltd Electrophotographic sensitive body
JPS59223436A (en) * 1983-06-03 1984-12-15 Fuji Xerox Co Ltd Photosensitive body of selenium-tellurium alloy

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008227036A (en) * 2007-03-12 2008-09-25 Fujifilm Corp Radiation plane detector

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