JPH03236056A - Method for forming and recovering superfine particle - Google Patents
Method for forming and recovering superfine particleInfo
- Publication number
- JPH03236056A JPH03236056A JP2033232A JP3323290A JPH03236056A JP H03236056 A JPH03236056 A JP H03236056A JP 2033232 A JP2033232 A JP 2033232A JP 3323290 A JP3323290 A JP 3323290A JP H03236056 A JPH03236056 A JP H03236056A
- Authority
- JP
- Japan
- Prior art keywords
- brush
- ultrafine particles
- superfine particles
- particles
- outside surface
- 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
- 238000000034 method Methods 0.000 title claims abstract description 22
- 239000002245 particle Substances 0.000 title abstract description 12
- 238000001704 evaporation Methods 0.000 claims abstract description 17
- 239000011882 ultra-fine particle Substances 0.000 claims description 35
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 239000000463 material Substances 0.000 abstract description 46
- 239000007789 gas Substances 0.000 abstract description 11
- 238000007790 scraping Methods 0.000 abstract description 11
- 238000011084 recovery Methods 0.000 abstract description 9
- 230000006866 deterioration Effects 0.000 abstract description 6
- 239000011261 inert gas Substances 0.000 abstract description 5
- 229920000049 Carbon (fiber) Polymers 0.000 abstract description 2
- 239000004917 carbon fiber Substances 0.000 abstract description 2
- 230000008020 evaporation Effects 0.000 description 10
- 108091008695 photoreceptors Proteins 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- 239000010410 layer Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 239000012860 organic pigment Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 238000003860 storage Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000049 pigment Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 1
- MCSXGCZMEPXKIW-UHFFFAOYSA-N 3-hydroxy-4-[(4-methyl-2-nitrophenyl)diazenyl]-N-(3-nitrophenyl)naphthalene-2-carboxamide Chemical compound Cc1ccc(N=Nc2c(O)c(cc3ccccc23)C(=O)Nc2cccc(c2)[N+]([O-])=O)c(c1)[N+]([O-])=O MCSXGCZMEPXKIW-UHFFFAOYSA-N 0.000 description 1
- 241000239290 Araneae Species 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- PGEHNUUBUQTUJB-UHFFFAOYSA-N anthanthrone Chemical compound C1=CC=C2C(=O)C3=CC=C4C=CC=C5C(=O)C6=CC=C1C2=C6C3=C54 PGEHNUUBUQTUJB-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000003779 heat-resistant material Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 238000004093 laser heating Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000011146 organic particle Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920003227 poly(N-vinyl carbazole) Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000003685 thermal hair damage Effects 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Landscapes
- 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、電子写真感光体の製造に当って用いる有機光
導電体超微粒子などを得る場合における超微粒子の生成
・回収方法と装置に係り、特にガス中蒸発法により超微
粒子を生成させこれを回収する方法に関する。ガス中蒸
発法とは、真空容器内に導入された不活性ガス雰囲気中
で種々の物質を加熱・蒸発・昇華させ、得られる蒸気分
子が不活性ガス分子と衝突しながら徐々に冷却され分子
同士が凝集し、超微粒子を形成させ、その超微粒子を回
収する方法である。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a method and apparatus for producing and collecting ultrafine particles when obtaining ultrafine organic photoconductor particles used in the production of electrophotographic photoreceptors. In particular, the present invention relates to a method for producing and recovering ultrafine particles by evaporation in gas. The in-gas evaporation method involves heating, evaporating, and sublimating various substances in an inert gas atmosphere introduced into a vacuum container, and the resulting vapor molecules collide with inert gas molecules to gradually cool down and cause the molecules to interact with each other. This is a method in which the particles are aggregated to form ultrafine particles, and the ultrafine particles are collected.
電子写真感光体は、導電性基体上に感光層を形成した基
本構造をもっている。この感光層を形成するための光導
電物質としては、従来、セレンを用いたものが一般的で
あり、その他無機光導電物質として硫化カドミウムや酸
化亜鉛等も知られている。An electrophotographic photoreceptor has a basic structure in which a photosensitive layer is formed on a conductive substrate. As a photoconductive material for forming this photosensitive layer, selenium has conventionally been commonly used, and other inorganic photoconductive materials such as cadmium sulfide and zinc oxide are also known.
しかし、近年では有機光導電物質を用いることによって
、成膜性の向上を図り、塗工によって生産することによ
り生産性を高める試みがなされている。また、有機光導
電物質を用いると、使用する染料や顔料等の増感剤を選
択すると、感色性を自在にコントロールできる利点があ
る。有機光導電物質としては、ポリ−Ｎ−ビニルカルバ
ゾールや２，５−ビス（Ｐ−ジエチルアミノフェニル）
−１、３．４−オキサジアゾール等が知られている。However, in recent years, attempts have been made to improve film formability by using organic photoconductive substances and to increase productivity by producing by coating. Further, when an organic photoconductive substance is used, there is an advantage that color sensitivity can be freely controlled by selecting a sensitizer such as a dye or a pigment to be used. Examples of organic photoconductive substances include poly-N-vinylcarbazole and 2,5-bis(P-diethylaminophenyl).
-1,3,4-oxadiazole and the like are known.
他方、近年、μｍまたは入オーダーの超微粒子に関して
の研究が種々なされている。かかる超微粒子は、その比
表面積が増大することによって、高い活性度を示すこと
に着目して生成させるものである。On the other hand, in recent years, various studies have been conducted on ultrafine particles of μm or small order. Such ultrafine particles are produced by focusing on the fact that they exhibit high activity by increasing their specific surface area.
この場合、中でもガス中蒸発法が注目を浴びている。従
来、この方法は専ら無機または金属材料の超微粒子を得
る場合について研究の指向性があったが、たとえば［機
能材料Ｊ １９８７年６月号、４４〜４９頁に記載の
ように、有機物超微粒子を得る場合にも研究がなされて
いる。In this case, the in-gas evaporation method is attracting attention. Conventionally, this method has been researched exclusively in the case of obtaining ultrafine particles of inorganic or metallic materials, but for example, as described in [Functional Materials J, June 1987 issue, pp. 44-49, ultrafine organic particles Research has also been done on obtaining .
何れにしても、従来、ガス中蒸発し被付着体に付着した
超微粒子の回収に際しては、第５図または第６図のよう
にしていた。In any case, conventionally, ultrafine particles that have evaporated in a gas and adhered to an object have been recovered as shown in FIG. 5 or 6.
すなわち、その第１の方法は、第５図ｆａ）のように、
蒸発性材料Ｍを収容する容器５０、被付着体としての平
板または曲板５１および必要により落下粉体の回収容器
５２を真空チャンバー（図示せず）内に配設し、この真
空チャンバー内に不活性ガスを送入するとともに、その
内部を真空状態に減圧している状態で、容器５０および
または蒸発性材料Ｍを加熱して蒸発させ、この蒸発した
材料を前記曲板５１に付着させ、その後（ｂ）のように
、曲板５１表面の付着材料層をブラシ５３などにより掻
き落として回収箱５４に回収するものである。That is, the first method is as shown in Figure 5 fa),
A container 50 for accommodating the evaporable material M, a flat plate or curved plate 51 as an adherend, and, if necessary, a collection container 52 for falling powder, are arranged in a vacuum chamber (not shown). While supplying the active gas, the container 50 and/or the evaporative material M are heated and evaporated while the inside thereof is reduced to a vacuum state, and this evaporated material is attached to the curved plate 51, and then As shown in (b), the adhered material layer on the surface of the curved plate 51 is scraped off with a brush 53 or the like and collected in a collection box 54.
第２の方法は、第６図（ａ）のように、被付着体として
プラスチックウェブ６０をリール６１から繰り出しなが
らり−ル６２に巻き取る過程で、そのウェブ６０の表面
に、第１の方法と同様な蒸発態様で、蒸発性材料Ｍを付
着させ、その回収に際しては、（ｂｌのように、ウェブ
６０を巻き取ったり一ル６２からウェブ６０を逆に巻き
出し、その過程で表面の付着した蒸発性材料Ｍをブラシ
などにより掻き取り回収箱５４に回収するものである。In the second method, as shown in FIG. 6(a), in the process of unwinding a plastic web 60 as an adherend from a reel 61 and winding it onto a reel 62, the first method is applied to the surface of the web 60. The evaporable material M is deposited in the same evaporation manner as in , and when it is recovered, the web 60 is wound up or reversely unwound from the roll 62 as shown in (bl), and in the process, the surface adhesion is removed. The evaporative material M is scraped off with a brush or the like and collected into a collection box 54.
しかし、前記第１の方法は、バッチ方式であるため、回
収板に経時的に粉体が順次積層され所定の厚さまで付着
がなされる。したがって、回収板をいかに冷却しても、
積層された粉体層が蒸発源からの放射熱を受けて、耐熱
性に劣る粉体の場合において特に熱劣化が激しい。また
、針状成長する材料の場合、蜘蛛の巣状（糸状）に粒子
が成長し、目的の超微粒子を得ることができない。しか
も、積層に際して余分な粒子が落下して良好に回収する
ことが困難となる。さらに、次記第２の方法と同様に、
付着と回収との２工程となるので、操作的に能率が悪い
。However, since the first method is a batch method, the powder is sequentially stacked on the collection plate over time until it reaches a predetermined thickness. Therefore, no matter how much the collection plate is cooled,
The stacked powder layers receive radiant heat from the evaporation source, and thermal deterioration is particularly severe in the case of powders with poor heat resistance. Furthermore, in the case of a material that grows in the form of needles, the particles grow in the form of a spider's web (thread-like), making it impossible to obtain the desired ultrafine particles. Moreover, during stacking, excess particles fall and are difficult to collect properly. Furthermore, similar to the second method below,
Since there are two steps, adhesion and recovery, the process is inefficient in terms of operation.
他方、第２の方法では、工程が２工程となることととも
に、リール間で付着材料を掻き落とすので、掻き落とし
が安定せず、かつウェブがプラスチックであるため強く
ブラシを当てることができず、掻き落とし難い。したが
って、回収作業性が悪いとともに、回収率が劣る。On the other hand, in the second method, there are two steps, and since the adhering material is scraped off between the reels, the scraping is not stable, and since the web is made of plastic, it is not possible to apply a strong brush to the web. Difficult to scrape off. Therefore, the collection efficiency is poor and the collection rate is poor.
一方、本出願人は、先に特願平１−１４３４７９号にお
いて、ドラム状被付着体に対してブレードを接触させな
がら付着超微粒子を掻き落とすことを提案したが、被付
着体が僅かにでもその取付ガタにより振動したり、また
被付着体の表面が真円でないと、被付着体に対するブレ
ード先端の接触および押圧力が変化し掻き取りムラを生
じる。On the other hand, the present applicant previously proposed in Japanese Patent Application No. 1-143479 that the attached ultrafine particles be scraped off while bringing a blade into contact with a drum-shaped object to be adhered, but even if the adhered object is slightly If the mounting play causes vibration, or if the surface of the object to be adhered to is not a perfect circle, the contact and pressing force of the blade tip against the object to be adhered will change, causing uneven scraping.
また、掻き取り性を高めるためにブレードを強く被付着
体に接触させようとしても、ブレードの材質的な限界な
どから、過度に強く押圧させるとブレードが撓むなどの
理由により、線圧を高くするには限界があった。さらに
、ブレードはある幅を有するものであるため、高精度に
加工しても、その先端は必ずしも直線でなく、若干の凹
凸は避けられない。その結果、掻き取りムラを根本的に
生じる。かくして、ブレードを用いる限り、掻き取り性
の向上には限界があり、場合により、超微粒子が被付着
体表面にフィルム状に残存するいわゆるフィルミング現
象がみられる。In addition, even if you try to bring the blade into strong contact with the object to improve scraping performance, due to the limitations of the material of the blade, if you press too hard, the blade will bend. There was a limit to what I could do. Furthermore, since the blade has a certain width, even if it is machined with high precision, its tip is not necessarily straight, and some unevenness is unavoidable. As a result, uneven scraping fundamentally occurs. Thus, as long as a blade is used, there is a limit to the improvement in scraping performance, and in some cases, a so-called filming phenomenon in which ultrafine particles remain in the form of a film on the surface of the adherend is observed.
そこで、本発明の主たる目的は、回収性にきわめて優れ
るとともに、回収効率が高く、回収する超微粒子の性状
が優れる超微粒子の生成・回収方法を提供することにあ
る６
〔課題を解決するための手段〕
上記課題は、ガス中蒸発法により蒸発した超微粒子を連
続的に回転する外面円筒の被付着体に付着させ、その被
付着体の回転過程で前記被付着体と軸を平行にした外面
円筒のブラシを前記被付着体表面に接触させて前記超微
粒子を連続的に掻き落として回収することで解決できる
。Therefore, the main purpose of the present invention is to provide a method for producing and recovering ultrafine particles that has extremely excellent recovery performance, high recovery efficiency, and excellent properties of the recovered ultrafine particles6. Means] The above-mentioned problem is achieved by attaching ultrafine particles evaporated by an in-gas evaporation method to a continuously rotating outer cylindrical adherend, and in the process of rotation of the adherend, the outer surface whose axis is parallel to the adherend. This problem can be solved by bringing a cylindrical brush into contact with the surface of the adherend to continuously scrape off and collect the ultrafine particles.
本発明では、外面円筒の被付着体を用い、これを回転さ
せる過程で、その表面に付着した超微粒子を掻き取るよ
うにしているので、付着した超微粒子が速やかに掻き落
とされ、蒸発源からの熱劣化などがなく性状・物性に優
れた超微粒子を得ることができるとともに、−工程で超
微粒子の生成および回収を行うことができる。In the present invention, an adherend with a cylindrical outer surface is used, and in the process of rotating it, the ultrafine particles adhering to the surface are scraped off, so that the adhered ultrafine particles are quickly scraped off and removed from the evaporation source. It is possible to obtain ultrafine particles with excellent properties and physical properties without thermal deterioration, and the ultrafine particles can be generated and recovered in the -step.
さらに、被付着体に付着した超微粒子の掻き落としに際
して、ブラシを用いており、これらの毛先を点的に被付
着体表面に抑圧できるので、十分な接触圧力を得ること
ができ、もって掻き落とし性が優れたものとなる。さら
に、被付着体およびブラシがそれぞれ外面円筒であるた
め、先に提案した例のように両者の接触面が平面である
ときと比較して、被付着体表面からブラシの毛先が離れ
たとき、超微粒子を跳ね飛ばす力が大きくなる。Furthermore, when scraping off the ultrafine particles adhering to the object, a brush is used, and since the tips of these bristles can be pressed onto the surface of the object in spots, sufficient contact pressure can be obtained, which makes it possible to scrape off the ultrafine particles that have adhered to the object. It has excellent removability. Furthermore, since the adherend and the brush each have a cylindrical outer surface, when the brush bristles are separated from the adherend surface, compared to when the contact surface between the two is flat as in the example proposed earlier, , the power to knock off ultrafine particles increases.
さらに、被付着体表面およびブラシの加工精度に左右さ
れないの。Furthermore, it is not affected by the surface of the object to be adhered to or the machining accuracy of the brush.
かかる理由により、掻き取り性が先の提案例に比較して
格段に優れたものとなる。For this reason, the scraping property is much better than that of the previously proposed example.
以下本発明をさらに詳説する。 The present invention will be explained in more detail below.
第１図は本発明の第１実施例を示したもので、真空チャ
ンバー１内に、蒸発性材料Ｍの収容容器２、外面円筒の
回転ドラム３およびこれに臨む一部が開口した回収箱４
が配設されている。真空チャンバー１にはアルゴンやヘ
リウムなどの不活性ガスＧの供給管５、真空ポンプ６に
連なる排気管７がそれぞれ連通しており、排気管７には
真空度を検出するための圧力計８が取付られている。回
転ドラム３は収容容器２の上方に位置して配置されてい
る。また、回収箱４は熱遮蔽材料により形成され、収容
容器２および回転ドラム３への蒸発性材料Ｍの付着部と
熱的に遮断されている。FIG. 1 shows a first embodiment of the present invention, in which a vacuum chamber 1 includes a container 2 for storing an evaporable material M, a rotating drum 3 with a cylindrical outer surface, and a collection box 4 facing the drum with a partially open part.
is installed. The vacuum chamber 1 is connected to a supply pipe 5 for an inert gas G such as argon or helium, and an exhaust pipe 7 connected to a vacuum pump 6. The exhaust pipe 7 is equipped with a pressure gauge 8 for detecting the degree of vacuum. It is installed. The rotating drum 3 is located above the container 2. The collection box 4 is made of a heat shielding material and is thermally isolated from the storage container 2 and the portion where the evaporative material M is attached to the rotating drum 3.
他方、回収箱４内には、ブラシロール９Ａの周囲に多数
のブラシ毛９Ｂを有する外面円筒ブラシ９が、回収箱４
の開口を介して回転ドラム３表面に接触するように、回
転ドラム３の回転軸と平行な回転軸をもって配設されて
いる。さらに、回転ドラム３は実施例では時計方向に図
示しない駆動モータにより回転されるようになっている
とともに、ブラシ９はブラシロール９Ａが図示しない駆
動モータにより同時計方向に回転するようになっている
。On the other hand, inside the collection box 4, an outer cylindrical brush 9 having a large number of bristles 9B around a brush roll 9A is placed inside the collection box 4.
The rotary drum 3 is disposed with a rotation axis parallel to the rotation axis of the rotary drum 3 so as to be in contact with the surface of the rotary drum 3 through an opening of the rotary drum 3 . Further, in the embodiment, the rotary drum 3 is rotated clockwise by a drive motor (not shown), and the brush roll 9A of the brush 9 is rotated in the same clockwise direction by a drive motor (not shown). .
また、ブラシ９のブラシ毛９Ｂの回転域において、振り
落としブレードｌＯが回収箱４に固定された状態で設け
られている。Further, in the rotation range of the bristles 9B of the brush 9, a shake-off blade 10 is provided fixed to the collection box 4.
さらに、蒸発性材料Ｍの収容容器２はセラミックなどの
耐熱性材料で形成しておくのが好ましく、この収容容器
２およびまたは直接蒸発性材料Ｍがヒーター加熱、誘導
加熱、レーザー加熱、抵抗加熱あるいは電子銃加熱など
によりその材料Ｍが充分蒸発する温度に加熱される。ま
た、その際、回転ドラム３は真空チャンバー１内の温度
にしておく他、好ましくは冷却、たとえば１０℃以下に
冷却しておく。この冷却には、回転ドラム３内に冷却用
熱媒体たとえば冷却水を通すことで可能である。Further, it is preferable that the storage container 2 for the evaporable material M is made of a heat-resistant material such as ceramic, and that the storage container 2 and/or the directly evaporable material M can be heated by heater heating, induction heating, laser heating, resistance heating or The material M is heated by electron gun heating or the like to a temperature at which the material M is sufficiently evaporated. Further, at this time, the rotating drum 3 is not only kept at the temperature within the vacuum chamber 1, but also preferably cooled, for example, to 10° C. or lower. This cooling can be achieved by passing a cooling heat medium, such as cooling water, through the rotating drum 3.
このように構成された装置において、真空チャンバー１
内を真空ポンプ６により減圧して高真空にした後、不活
性ガスを送入し、好ましくは０．０１〜５０ Ｔｏｒｒ
に保つ。この状態で、蒸発性材料Ｍに対して加熱すると
、そのガス中蒸発が生じ、蒸発した材料Ｍは、回転して
いる回転ドラム３の表面に連続的に付着する。この付着
した材料Ｍは、接触部において向流的に接触するブラシ
９により掻き取られ回収箱４内に回収される。また、ブ
ラシ毛９Ｂに付着した材料Ｍについては、ブレードｌＯ
に毛先が接触するので、同様に掻き取られる。In the apparatus configured in this way, the vacuum chamber 1
After reducing the pressure inside the chamber to a high vacuum using the vacuum pump 6, an inert gas is introduced, preferably at a pressure of 0.01 to 50 Torr.
Keep it. In this state, when the evaporative material M is heated, evaporation occurs in the gas, and the evaporated material M continuously adheres to the surface of the rotating drum 3. This adhered material M is scraped off by the brush 9 that contacts countercurrently at the contact portion and is collected into the collection box 4 . Moreover, regarding the material M attached to the brush bristles 9B, the blade lO
Since the tips of the hair come into contact with the , it is scraped off in the same way.
材料Ｍが掻き取られ裸になった回転ドラム３の表面には
次の新たな材料が付着される。このようにして、回転ド
ラム３の表面において、材料Ｍの付着および掻き取りが
連続的になされる。したがって、回転ドラム３の表面に
付着した材料は速やかに、再び材料加熱用熱源からの輻
射熱を受けることな（掻き取られるので、従来の第１法
のように、熱による劣化（熱ダメージ）がなく、良質な
超微粒子を得ることができる。蒸発付着から掻き取りま
での時間は、たとえば回転ドラム３の回転速度を調節す
ることが設定できる。The next new material is adhered to the surface of the rotary drum 3 from which the material M has been scraped off and becomes bare. In this way, the material M is continuously deposited and scraped off on the surface of the rotating drum 3. Therefore, the material adhering to the surface of the rotating drum 3 is quickly scraped off without being exposed to radiant heat from the heat source for heating the material again, so unlike the conventional first method, there is no deterioration due to heat (thermal damage). The time from evaporation deposition to scraping can be set by adjusting the rotational speed of the rotary drum 3, for example.
回収箱４に回収された超微粒子は、ある程度の量となっ
た時点で、ガス中蒸発操作を終了して、真空チャンバー
■を開放して取り出される。When the ultrafine particles collected in the collection box 4 reach a certain amount, the evaporation operation in the gas is completed, the vacuum chamber (2) is opened, and the ultrafine particles are taken out.
第２図は第２実施例を示したもので、回転ドラム３に対
して、複数図示例では２つのブラシ９Ｘ、９Ｙを配設し
たものである。この場合、ブラン９Ｙによる掻き取り力
をブラシ９Ｘの掻き取り力より大きくすることができる
。FIG. 2 shows a second embodiment, in which two brushes 9X and 9Y are disposed on the rotary drum 3 in the illustrated example. In this case, the scraping force by the swing 9Y can be made larger than the scraping force by the brush 9X.
ブラシ毛９Ｂの材質、植設密度、高さ、太さなどは適宜
選定できる。材質としては、通常金属繊維を用いるが、
もし、材料Ｍが静電気を発生させブラシに付着しがちの
場合、ブラシ毛９Ｂの材質としてカーボン繊維を用いる
ことができる。ブラシ毛９Ｂの毛先形状は、球状より第
３図のように各張っているのが望ましい。回転ドラム３
の材質としでは、適宜のものを用いることができるが、
通常、金属製のものを用いることができる。The material, planting density, height, thickness, etc. of the brush bristles 9B can be selected as appropriate. Metal fiber is usually used as the material, but
If the material M generates static electricity and tends to adhere to the brush, carbon fiber can be used as the material for the brush bristles 9B. It is preferable that the tips of the brush bristles 9B have a taut shape as shown in FIG. 3 rather than a spherical shape. Rotating drum 3
As for the material, any suitable material can be used, but
Usually, metal can be used.
ブラシ９に付着した材料Ｍを振るい落とすには、第４図
のように、振るい落とし糸１１をブラシ毛９Ｂの回転域
に張設することができる。In order to shake off the material M adhering to the brush 9, a sieving thread 11 can be stretched over the rotating region of the brush bristles 9B, as shown in FIG.
他方、回転ドラム３からの材料Ｍの掻き落とし性を高め
るために、ブラシ９を回転トラム３表面に対して接離す
る、あるいは回転ドラム３の軸方向と平行に往復運動す
るように振動させることができる。On the other hand, in order to improve the ability to scrape off the material M from the rotating drum 3, the brush 9 may be moved toward and away from the surface of the rotating tram 3, or vibrated so as to reciprocate in parallel to the axial direction of the rotating drum 3. I can do it.
上記各側では、蒸発性材料を収容容器にバッチ的に供給
したが、真空チャンバー内の加熱容器へスクリューフィ
ーダーなどにより連続的に供給するなどすれば大量の蒸
発処理が可能である。In each of the above-mentioned sides, the evaporable material was supplied to the storage container in a batch manner, but a large amount of evaporation processing can be performed by continuously supplying the evaporable material to the heating container in the vacuum chamber using a screw feeder or the like.
本発明において、目的の超微粒子としては、１０〜数万
人、特に１０〜数千人を得る場合において好適に適用で
きる。また、超微粒子の種類としては、無機材料、金属
材料の他、有機材料であってもよい。特に、本発明者ら
は、有機感光体を得る場合の有機顔料、とりわけアンス
アンスロン系顔料を得る場合に最適であることを確認済
である。In the present invention, the target ultrafine particles can be suitably applied when obtaining 10 to tens of thousands of people, particularly 10 to several thousand people. Further, the type of ultrafine particles may be an organic material as well as an inorganic material or a metal material. In particular, the present inventors have confirmed that it is optimal for obtaining organic pigments, particularly anth-anthrone pigments, for obtaining organic photoreceptors.
有機感光体は、導電性基体上に、有機光導電体粒子を、
分散機によって分散剤およびバインダー樹脂中に分散し
たものを塗布することにより一般的に得ることができる
。Organophotoreceptors include organic photoconductor particles on a conductive substrate.
It can generally be obtained by coating a dispersant dispersed in a dispersant and a binder resin using a dispersing machine.
この場合、最終的に得ようとする感光体としては、導電
性基体上に、有機光導電体粒子（顔料）を電荷発生材料
として電荷輸送材料中に分散させた単一層型感光体と、
導電性基体上に、電荷発生材料層を形成しその上に電荷
輸送材料層を形成した機能分離型感光体とがある。本発
明は、これら両者の形態の感光体の製造における超微粒
子を得る場合に適している。In this case, the final photoreceptor to be obtained is a single-layer photoreceptor in which organic photoconductor particles (pigment) are dispersed in a charge transport material as a charge generation material on a conductive substrate;
There is a functionally separated photoreceptor in which a charge-generating material layer is formed on a conductive substrate and a charge-transporting material layer is formed thereon. The present invention is suitable for obtaining ultrafine particles in the production of photoreceptors of both types.
次に実施例を示し本発明の効果を明らかにする。 Next, Examples will be shown to clarify the effects of the present invention.
（実施例１） 第１図の装置により、ガス中蒸発を行った。(Example 1) Evaporation in gas was performed using the apparatus shown in FIG.
電子写真用有機感光体を製造するために用いる有機顔料
超微粒子を生成・回収した。この有機顔料としては、４
．ｌＯ−ジブロモアンスアンスロンを用い、真空チャン
バーをヘリウムガス雰囲気下に置き、かつ１Ｏ＝Ｔｏｒ
ｒに減圧し、材料を３００〜３５０℃に加熱し真空蒸発
させ第１図法に従って超微粒子を得た。Ultrafine organic pigment particles used for manufacturing organic photoreceptors for electrophotography were produced and recovered. As this organic pigment, 4
．． Using 1O-dibromoanthron, the vacuum chamber is placed under a helium gas atmosphere, and 1O=Tor
The material was heated to 300 to 350°C and evaporated in vacuum to obtain ultrafine particles according to the method shown in Figure 1.
その結果、熱劣化がない超微粒子を約４５％の回収率を
もって回収できた。また、この回収率は回転ドラムの径
、蒸発率を制御することでほぼ１００％の回収率が得ら
れることが他の実験により明らかとなった。As a result, ultrafine particles without thermal deterioration could be recovered with a recovery rate of about 45%. Further, other experiments have revealed that a recovery rate of approximately 100% can be obtained by controlling the diameter of the rotating drum and the evaporation rate.
（比較例１）
第５図の従来法１によって、同様の有機顔料を得た。そ
の結果、回収した粉体は糸状となり、かつその内部は、
オレンジ色、表面は深紅色となっており、熱劣化の影響
が明らかに認められ、回収率は３５〜４０％であった。(Comparative Example 1) A similar organic pigment was obtained by conventional method 1 shown in FIG. As a result, the collected powder becomes thread-like, and its inside is
The color was orange, and the surface was deep red, and the influence of thermal deterioration was clearly recognized, and the recovery rate was 35 to 40%.
（比較例２）
第６図の従来法２によって、同様の有機顔料を回収した
。その結果、超微粒子を得ることができたが、比較例１
の場合の２００倍の時間（延べ５０時間）の操作時間を
要し、かつ回収率は６〜７％と著しく低かった。(Comparative Example 2) A similar organic pigment was recovered by conventional method 2 shown in FIG. As a result, ultrafine particles could be obtained, but Comparative Example 1
The operation time was 200 times longer (total of 50 hours) than in the case of the above method, and the recovery rate was extremely low at 6 to 7%.
以上の通り、本発明によれば、回収性にきわめて優れる
とともに、回収効率が高く、回収する超微粒子の性状が
優れる超微粒子を生成・回収できる。As described above, according to the present invention, it is possible to generate and recover ultrafine particles that have extremely excellent recoverability, high recovery efficiency, and excellent properties of the recovered ultrafine particles.
第１図は本発明の第１実施例の概要図、第２図は第２実
施例の概要図、第３図はブラシ毛の形状例の拡大図、第
４図はブラシ毛に付着した超微粒子の振るい落とし線の
配設例の概要図、第５図および第６図はそれぞれ従来技
術の概要説明図である。FIG. 1 is a schematic diagram of the first embodiment of the present invention, FIG. 2 is a schematic diagram of the second embodiment, FIG. 3 is an enlarged diagram of an example of the shape of the brush bristles, and FIG. A schematic diagram of an example of arrangement of drop lines for fine particles, and FIGS. 5 and 6 are schematic explanatory diagrams of the prior art, respectively.
Claims (2)
回転する外面円筒の被付着体に付着させ、その被付着体
の回転過程で前記被付着体と軸を平行にした外面円筒の
ブラシを前記被付着体表面に接触させて前記超微粒子を
連続的に掻き落として回収することを特徴とする超微粒
子の生成・回収方法。(1) Ultrafine particles evaporated by the in-gas evaporation method are attached to a continuously rotating external cylindrical object, and the external cylindrical brush whose axis is parallel to the adhering object during the rotation process of the adhering object. A method for producing and collecting ultrafine particles, characterized in that the ultrafine particles are continuously scraped off and recovered by bringing the ultrafine particles into contact with the surface of the adherend.
請求項１記載の方法。(2) The method according to claim 1, wherein the object to be adhered and the brush are rotated in the same direction.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2033232A JPH03236056A (en) | 1990-02-14 | 1990-02-14 | Method for forming and recovering superfine particle |
| US07/592,366 US5374382A (en) | 1990-02-14 | 1990-10-03 | Method of generation and recovery of ultra-fine particles |
| DE4031898A DE4031898C2 (en) | 1990-02-14 | 1990-10-08 | Process for producing and recovering ultrafine particles |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2033232A JPH03236056A (en) | 1990-02-14 | 1990-02-14 | Method for forming and recovering superfine particle |
| US07/592,366 US5374382A (en) | 1990-02-14 | 1990-10-03 | Method of generation and recovery of ultra-fine particles |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH03236056A true JPH03236056A (en) | 1991-10-22 |
Family
ID=26371904
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2033232A Pending JPH03236056A (en) | 1990-02-14 | 1990-02-14 | Method for forming and recovering superfine particle |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03236056A (en) |
-
1990
- 1990-02-14 JP JP2033232A patent/JPH03236056A/en active Pending
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