JPH0463130A - Method for forming and recovering superfine particles - Google Patents
Method for forming and recovering superfine particlesInfo
- Publication number
- JPH0463130A JPH0463130A JP17212690A JP17212690A JPH0463130A JP H0463130 A JPH0463130 A JP H0463130A JP 17212690 A JP17212690 A JP 17212690A JP 17212690 A JP17212690 A JP 17212690A JP H0463130 A JPH0463130 A JP H0463130A
- Authority
- JP
- Japan
- Prior art keywords
- vacuum chamber
- ultrafine particles
- evaporating material
- inert gas
- evaporating
- 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
- 239000002245 particle Substances 0.000 title abstract description 14
- 238000000034 method Methods 0.000 title description 13
- 239000000463 material Substances 0.000 claims abstract description 48
- 239000011261 inert gas Substances 0.000 claims abstract description 10
- 238000007664 blowing Methods 0.000 claims abstract 3
- 239000011882 ultra-fine particle Substances 0.000 claims description 26
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 abstract description 24
- 230000008020 evaporation Effects 0.000 abstract description 7
- 238000011084 recovery Methods 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract 3
- 239000007789 gas Substances 0.000 description 11
- 108091008695 photoreceptors Proteins 0.000 description 8
- 230000002265 prevention Effects 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- 239000010410 layer Substances 0.000 description 5
- 238000003860 storage Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000012860 organic pigment Substances 0.000 description 3
- 239000000049 pigment Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000007790 scraping Methods 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
- 239000011230 binding agent Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 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
- 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
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000003779 heat-resistant material Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 238000004093 laser heating Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000011146 organic particle Substances 0.000 description 1
- 229920003227 poly(N-vinyl carbazole) Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 230000003685 thermal hair damage Effects 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Landscapes
- Photoreceptors In Electrophotography (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Glanulating (AREA)
- Physical Or Chemical Processes And Apparatus (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
・回収方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for producing and recovering ultrafine particles of organic photoconductors used in the production of electrophotographic photoreceptors.
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または人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 on the micrometer or human order. Such ultrafine particles are produced by focusing on the fact that they exhibit high activity by increasing their specific surface area.
一般に、超微粒子を得るまたはこれを基材表面に付着さ
せる場合の手法として、気相生成法（電気炉法、化学炎
法、プラズマ法、ガス中蒸発法）、液相生成法（沈澱法
、溶媒蒸発法）、あるいは物理的粉砕法（サンドミル、
ボールミル、アトライターなどを用いる）などがある。Generally, methods for obtaining ultrafine particles or attaching them to the surface of a substrate include gas phase generation methods (electric furnace method, chemical flame method, plasma method, evaporation method in gas), liquid phase generation methods (precipitation method, (solvent evaporation method) or physical grinding method (sand mill,
(using a ball mill, attritor, etc.).
一般に、高真空中で材料を蒸発させ、これを基材へ付着
させると、蒸着膜となり、粉体として回収できないが、
前記のガス中蒸発法は、超微粒子として回収できる利点
を有するなどの理由により注目を浴びている。このガス
中蒸発法とは、１０−”〜１０ ”Ｔｏｒｒの範囲内に
保持された真空容器内に、不活性ガスを導入し、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。Generally, when a material is evaporated in a high vacuum and attached to a substrate, it becomes a vapor deposited film that cannot be recovered as a powder.
The above-mentioned in-gas evaporation method is attracting attention because it has the advantage of being able to recover ultrafine particles. This in-gas evaporation method involves introducing an inert gas into a vacuum container maintained within a range of 10 to 10 Torr, and heating, evaporating, and sublimating various substances in the inert gas atmosphere. This is a method in which the obtained vapor molecules are gradually cooled while colliding with inert gas molecules, causing the molecules to coagulate, forming ultrafine particles, and recovering the ultrafine particles.
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。Conventionally, this method has been research-oriented exclusively for obtaining ultrafine particles of inorganic or metallic materials, but for example,
As described in Functional Materials J, June 1987 issue, pages 44-49, research has also been conducted to obtain ultrafine organic particles.
しかし、前記のガス中蒸発法は、超微粒子を好適に回収
できる点で、他の気相生成法に比較して有効であるが、
アルゴンやヘリウムなどの不活性ガスを真空チャンバー
内の吹込みながら、他方でこれを真空排気ポンプにより
排気することを必要とし、不活性ガスの吹込み・排気設
備の経済的負担が大きく、運転費も嵩むものであった。However, the above-mentioned in-gas evaporation method is more effective than other gas-phase generation methods in that ultrafine particles can be recovered appropriately;
While injecting an inert gas such as argon or helium into the vacuum chamber, it is also necessary to exhaust it with a vacuum pump, which imposes a large economic burden on the inert gas injection and exhaust equipment, and increases operating costs. It was also bulky.
しかも、粒子径を小さくするために、真空チャンバー内
の圧力を徐々に低下させて行くと、粉体の状態での回収
が不可能になり、逐には蒸着膜しか得られないでいた。Moreover, if the pressure inside the vacuum chamber was gradually lowered in order to reduce the particle size, it became impossible to recover the powder in the form of a powder, and in the end only a vapor-deposited film could be obtained.
したがって、本発明の課題は、簡素な設備の下で、安価
かつ確実により粒子径の小さい超微粒子を回収すること
にある。Therefore, an object of the present invention is to inexpensively and reliably recover ultrafine particles with small particle diameters using simple equipment.
上記課題は、真空チャンバー内に蒸発性材料を収納する
とともに、この蒸発性材料の近くに被付着体を配設し、
前記蒸発性材料を加熱し、前記被付着体の少なくとも表
面温度を前記蒸発性材料より低温とし、前記真空チャン
バー内の圧力を１Ｏ−ｊＴｏｒｒ以下とし、かつその内
部に不活性ガスの吹込みを行うことなく、前記蒸発性材
料の蒸発を行い、被付着体に付着した材料をその表面か
ら除去して回収することで解決できる。The above problem is solved by storing an evaporative material in a vacuum chamber, and arranging an adherend near the evaporative material.
The vaporizable material is heated, at least the surface temperature of the adherend is lower than that of the vaporizable material, the pressure in the vacuum chamber is set to 1 O-jTorr or less, and an inert gas is blown into the vacuum chamber. This problem can be solved by evaporating the evaporable material and removing the material adhering to the object from its surface and recovering it.
本発明に従って、真空チャンバー内の圧力を、従来のガ
ス中蒸発法の真空度が高い、１０−−３Ｔｏｒｒ以下の
高真空に維持すると、不活性ガスの吹込み・排気を行わ
ない条件の下で、超微粒子を回収できるとともに、より
小さい超微粒子を得ることができる。According to the present invention, if the pressure inside the vacuum chamber is maintained at a high vacuum of 10-3 Torr or less, which is the high degree of vacuum in the conventional in-gas evaporation method, the , ultrafine particles can be recovered and smaller ultrafine particles can be obtained.
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には真空ポンプ５に連
なる排気管６がそれぞれ連通している。真空チャンバー
１内には真空度を検出するための圧力計７が取付られて
いる。FIG. 1 shows an embodiment of the present invention, in which a container 2 for storing an evaporative material M, a rotating drum 3 having a cylindrical outer surface, and a collection box 4 facing the drum with a partially open side are arranged in a vacuum chamber 1. It is set up. Exhaust pipes 6 connected to vacuum pumps 5 communicate with the vacuum chamber 1, respectively. A pressure gauge 7 is installed inside the vacuum chamber 1 to detect the degree of vacuum.
また、前記回転ドラム３は収容容器２の上方に位置して
配置されている。さらに、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。Furthermore, the rotating drum 3 is located above the container 2 . Further, the collection box 4 is formed 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８Ａの周囲に多数
のブラシ毛８Ｂを有する外面円筒ブラシ８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８はブラシロール８Ａ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 8 having a large number of bristles 8B around a brush roll 8A 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 rotating drum 3 is rotated clockwise by a drive motor (not shown), and the brush roll 8A of the brush 8 is rotated in the same clockwise direction by a drive motor (not shown). .
また、ブラシ８のブラシ毛８Ｂの回転域において、振り
落とし板９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 8B of the brush 8, a shake-off plate 9 is provided in a state 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.
一方、本発明の好ましい実施例においては、収容容器２
から被付着体すなわち回転ドラム３に延在して蒸発した
超微粒子の回転ドラム３へ向かう方向以外の飛散を防止
するための飛散防止壁１０が設けられている。第１図の
飛散防止壁ｌＯの上端は、回転ドラム３に近接している
。また、この飛散防止壁工０には、加熱ヒータ１１が取
り付けられ、飛散防止壁１０を加熱するようにしである
。On the other hand, in a preferred embodiment of the present invention, the storage container 2
A scattering prevention wall 10 is provided to prevent ultrafine particles that have evaporated from the object to be adhered to and evaporated from scattering in a direction other than the direction toward the rotating drum 3. The upper end of the scattering prevention wall lO in FIG. 1 is close to the rotating drum 3. Further, a heater 11 is attached to this scattering prevention wall work 0 to heat the scattering prevention wall 10.
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５により減圧して、１Ｏ−３Ｔｏｒｒ以
下、より好ましくは１０ −３Ｔｏｒｒ以下の高真空に
される。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の表面に主に温度差により連続的に付
着する。In the apparatus configured in this way, the vacuum chamber 1
The internal pressure is reduced by the vacuum pump 5 to create a high vacuum of 10-3 Torr or less, more preferably 10-3 Torr or less. When the evaporative material M is heated in this state, evaporation occurs in the gas, and the evaporated material M continuously adheres to the surface of the rotating drum 3 mainly due to the temperature difference.
かくして、回転ドラム３表面に付着した材料Ｍは、接触
部において向流的に接触するブラシ８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８Ｂに付着し
た材料Ｍについては、掻き落とし板９に毛先が接触する
ので、同様に掻き取られる。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。In this way, the material M adhering to the surface of the rotating drum 3 is scraped off by the brush 8 that contacts countercurrently at the contact portion and is collected into the collection box 4. Further, the material M attached to the brush bristles 8B is similarly scraped off since the tips of the bristles come into contact with the scraping plate 9. 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.
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
く掻き取られるので、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。Therefore, the material adhering to the surface of the rotating drum 3 is quickly scraped off without receiving radiant heat from the heat source for heating the material again, so there is no deterioration due to heat (thermal damage) and it is possible to obtain high-quality ultrafine particles. can. The time from evaporation deposition to scraping can be set, for example, by adjusting the rotation speed of the rotary drum 3.
回収箱４に回収された超微粒子は、ある程度の量となっ
た時点で操作を終了して、真空チャンバー１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 operation is finished, the vacuum chamber 1 is opened, and the ultrafine particles are taken out.
本発明において、被付着体としては、前記実施例の回転
ドラム３に代えて、連続搬送されるベルトや、位置固定
の被付着板なども用いることができる。In the present invention, as the object to be adhered to, a continuously conveyed belt, a fixed-position adherend plate, or the like may be used instead of the rotating drum 3 of the above embodiment.
また、被付着体に付着した超微粒子の回収手段としては
、ブラシのほか、ブレードによる掻き取り、ワイピング
クロスによる拭き取りなどの手段を用いることができる
。In addition to a brush, other means such as scraping with a blade or wiping with a wiping cloth can be used to collect the ultrafine particles adhering to the object.
さらに、上記例は連続的に超微粒子の付着および回収を
図るものであるが、バッチ式に付着・回収を図るように
してもよい。Further, in the above example, the ultrafine particles are continuously attached and recovered, but the attachment and recovery may be carried out in a batch manner.
ところで、前述の飛散防止壁１０の少なくとも内面の温
度は、たとえば加熱ヒータ１１により加熱し、蒸発源の
温度と同一、もしくはそれ以上の温度に加熱する。By the way, the temperature of at least the inner surface of the above-mentioned scattering prevention wall 10 is heated by, for example, the heater 11 to a temperature equal to or higher than the temperature of the evaporation source.
また、被付着体の温度は、蒸発源温度（蒸発性材料温度
）および飛散防止壁ｌＯの温度未満であり、かつ超微粒
子が充分熱沈着温度以下である範囲内において、可能な
限り低温であり、もって蒸発源温度と被付着体との間に
大きな熱勾配を採るのが望まれる。In addition, the temperature of the adherend should be as low as possible within a range that is below the evaporation source temperature (evaporative material temperature) and the scattering prevention wall lO temperature, and within the range where the ultrafine particles are sufficiently below the thermal deposition temperature. Therefore, it is desirable to create a large thermal gradient between the evaporation source temperature and the adherend.
このような温度の設定は、基本的には、対象の材料の種
類に依存するので、これに応じて適切に設定される。Such temperature settings basically depend on the type of material to be used, so they are appropriately set accordingly.
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。特に、粒子径として、従来のガス中蒸発法より小
さいものを得ることができる。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. In particular, it is possible to obtain smaller particle sizes than in conventional gas evaporation methods.
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流である
。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 the present invention 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、
分散機によってバインダー樹脂中に分散したものやその
他の層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 binder resin dispersed in a binder resin or another layer 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.
第１図の装置により、ガス中蒸発を行った。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
．１０−ジブロモアンスアンスロンを用い、これを５０
ｇ仕込み、真空チャンバーを１０−−３Ｔｏｒｒに減圧
し、材料を３００〜３５０℃に加熱し全量真空蒸発させ
、これを回転数１Ｏｒｐｍで回転する回転ドラムに連続
的に付着させ、これをブラシにより掻き取り、２０ｇの
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 10-dibromoanthrone, this
g, reduce the pressure in the vacuum chamber to 10-3 Torr, heat the material to 300 to 350°C, vacuum evaporate the entire amount, deposit it continuously on a rotating drum rotating at a rotation speed of 1 Orpm, and scrape it with a brush. 20 g of ultrafine particles were obtained.
また、得られた超微粒子をＴＥＭ観察したところ、粒径
がｄ、。＝０．０５〜０，０９μｍの極めて小さなもの
であることが確認された。なお、従来のガス中蒸発法に
より得られる粒子の粒径は、ｄ、。−０，０７μｍであ
る。Furthermore, when the obtained ultrafine particles were observed using a TEM, the particle size was d. It was confirmed that the particle size was extremely small, 0.05 to 0.09 μm. Note that the particle size of particles obtained by the conventional evaporation method in gas is d. -0.07 μm.
以上の通り、本発明によれば、簡素な設備の下で、安価
かつ確実に、従来のガス中蒸発法に比較してより粒子径
の小さい超微粒子を回収することができる。As described above, according to the present invention, ultrafine particles having a smaller particle size can be recovered inexpensively and reliably using simple equipment compared to the conventional evaporation method in gas.
第１図は本発明の実施例の概要図である。
１・・・真空チャンバー ２・・・収容容器、３・・・
回転ドラム、４・・・回収箱、５・・・真空ポンプ、８
・・・ブラシ、Ｍ・・・蒸発性材料、Ｇ・・・不活性ガ
ス特許出願人 コニカ株式会社−、〜、FIG. 1 is a schematic diagram of an embodiment of the present invention. 1... Vacuum chamber 2... Storage container, 3...
Rotating drum, 4... Collection box, 5... Vacuum pump, 8
...Brush, M...Evaporable material, G...Inert gas Patent applicant Konica Corporation -, ~,
Claims (1)
に、この蒸発性材料の近くに被付着体を配設し、前記蒸
発性材料を加熱し、前記被付着体の少なくとも表面温度
を前記蒸発性材料より低温とし、前記真空チャンバー内
の圧力を１０＾−＾３Ｔｏｒｒ以下とし、かつその内部
に不活性ガスの吹込みを行うことなく、前記蒸発性材料
の蒸発を行い、被付着体に付着した材料をその表面から
除去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) Storing an evaporative material in a vacuum chamber, disposing an adherend near the evaporative material, heating the evaporative material, and adjusting at least the surface temperature of the adherend to the evaporative material. The vaporizable material is evaporated at a lower temperature than the material, the pressure in the vacuum chamber is 10^-^3 Torr or less, and without blowing an inert gas into the vacuum chamber, and the material adheres to the adherend. A method for producing and collecting ultrafine particles, characterized by removing and collecting materials from their surfaces.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17212690A JPH0463130A (en) | 1990-06-29 | 1990-06-29 | Method for forming and recovering superfine particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17212690A JPH0463130A (en) | 1990-06-29 | 1990-06-29 | Method for forming and recovering superfine particles |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0463130A true JPH0463130A (en) | 1992-02-28 |
Family
ID=15936043
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP17212690A Pending JPH0463130A (en) | 1990-06-29 | 1990-06-29 | Method for forming and recovering superfine particles |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0463130A (en) |
-
1990
- 1990-06-29 JP JP17212690A patent/JPH0463130A/en active Pending
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