JPH0753236B2 - Ultrafine particle manufacturing method - Google Patents
Ultrafine particle manufacturing methodInfo
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- JPH0753236B2 JPH0753236B2 JP1225059A JP22505989A JPH0753236B2 JP H0753236 B2 JPH0753236 B2 JP H0753236B2 JP 1225059 A JP1225059 A JP 1225059A JP 22505989 A JP22505989 A JP 22505989A JP H0753236 B2 JPH0753236 B2 JP H0753236B2
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- crucible
- ultrafine particles
- raw material
- target substance
- substrate
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Description
【発明の詳細な説明】 ［産業上の利用分野］ 本発明は、超微粒子の製造方法に関し、特に水性溶媒等
の溶媒に対して優れた溶解性・分散性を有する超微粒子
を製造する方法に関する。TECHNICAL FIELD The present invention relates to a method for producing ultrafine particles, and more particularly to a method for producing ultrafine particles having excellent solubility and dispersibility in a solvent such as an aqueous solvent. .
［従来の技術］ 第２図を参照して、従来技術による超微粒子の作成方法
を説明する。[Prior Art] With reference to FIG. 2, a method for producing ultrafine particles according to the prior art will be described.
真空容器で形成される反応室１は、弁7,8を介して排気
系２と不活性ガス源３とに接続されている。反応容器１
の内部には原料を蒸発させるためのるつぼ４が配置さ
れ、るつぼ４上方には生成した超微粒子を付着させるた
めの基板５が配置されている。基板５は液体窒素系等の
冷却系（図示せず）によって冷却される。A reaction chamber 1 formed of a vacuum container is connected to an exhaust system 2 and an inert gas source 3 via valves 7 and 8. Reaction vessel 1
A crucible 4 for evaporating the raw material is arranged inside the, and a substrate 5 for adhering the generated ultrafine particles is arranged above the crucible 4. The substrate 5 is cooled by a cooling system (not shown) such as a liquid nitrogen system.
超微粒子作成においては、まず有機化合物等の所定組成
の原料をるつぼ４に仕込み、反応室１を気密に封じる。In producing ultrafine particles, first, a raw material having a predetermined composition such as an organic compound is charged into the crucible 4 and the reaction chamber 1 is hermetically sealed.
反応室１内を弁７を介して排気系２で、たとえば10−6T
orr位の高真空に排気した後、ヘリウム（He）、アルゴ
ン（Ar）等の不活性ガスを不活性ガス源３から弁８を介
して導入し、所定の不活性ガス圧とする。The reaction chamber 1 through the valve 7 in the exhaust system 2, for example 10- 6 T
After evacuating to a high vacuum of the orr level, an inert gas such as helium (He) or argon (Ar) is introduced from the inert gas source 3 through the valve 8 to a predetermined inert gas pressure.
その後、基板５を冷却し、あらかじめ原料を仕込んだる
つぼ４を徐々に加熱し、蒸発温度まで昇温する。加熱さ
れた原料は液化し、表面から気化・蒸発する。なお、原
料によっては、液化せず、固相から直接気相に昇華す
る。After that, the substrate 5 is cooled, and the crucible 4 charged with the raw materials in advance is gradually heated to raise the temperature to the evaporation temperature. The heated raw material is liquefied and vaporized and evaporated from the surface. Depending on the raw material, it does not liquefy, but sublimates directly from the solid phase to the gas phase.
るつぼ４で加熱され、蒸発した原料ガス分子は雰囲気の
不活性ガス分子と衝突して冷却され、徐々に凝集して超
微粒子を形成する。生成した超微粒子は、るつぼ４上方
に設置し、冷却した基板５に付着され、回収される。The raw material gas molecules heated and vaporized in the crucible 4 collide with the inert gas molecules in the atmosphere, are cooled, and are gradually aggregated to form ultrafine particles. The generated ultra-fine particles are placed above the crucible 4 and attached to the cooled substrate 5 to be collected.
有機物超微粒子のバルク粒子にする長所として、粒径の
減少に伴う表面電荷の変化および溶媒に対する溶解速度
ないしは分散性の向上がある。The advantage of using bulk particles of organic ultrafine particles is that the surface charge changes as the particle size decreases and the dissolution rate or dispersibility in a solvent improves.
物質の溶媒に対する溶解速度、過飽和度、分散性を決定
する重要なパラメータとして、粒径および粒子の結晶性
がある。有機物超微粒子は、バルク材に比較してその粒
径が著しく小さく、優れた溶解性（溶解速度、過飽和
度）ないし分散性を示す。Particle size and crystallinity of particles are important parameters that determine the dissolution rate, supersaturation degree, and dispersibility of a substance in a solvent. The organic ultrafine particles have a remarkably small particle size as compared with the bulk material, and exhibit excellent solubility (dissolution rate, supersaturation degree) or dispersibility.
一方、非晶質物質が、結晶性物質に比較して優れた溶解
性・分散性を示すことも良く知られている。On the other hand, it is well known that an amorphous substance has excellent solubility and dispersibility as compared with a crystalline substance.
従来、難溶性の薬品は、バルク原料と薬品添加物（乳
糖、メチルセルロース等）を混合し、ボールミル等で粉
砕、混合することで、超微粒子化するとともに非晶質性
を付与し、溶解性を高めていた。Conventionally, for sparingly soluble chemicals, bulk raw materials and chemical additives (lactose, methylcellulose, etc.) are mixed, pulverized and mixed with a ball mill, etc. to make them ultrafine particles and to impart amorphousness to improve solubility. It was high.
［発明が解決しようとする課題］ 以上述べたように、従来ある種の有機物に対して、溶媒
に対する溶解性・分散性を高めるため、ボールミル等で
超微粒子化することが行われた。しかし、ある種の有機
物においては、超微粒子化しても、精製する超微粒子の
結晶性が高く、期待した程の溶媒に対する溶解速度や過
飽和度の溶解性（あるいは分散性）の向上効果が得られ
ないことがあった。[Problems to be Solved by the Invention] As described above, in order to enhance the solubility and dispersibility in a solvent of a certain kind of organic substance, it has been conventionally made into ultrafine particles by a ball mill or the like. However, for some organic substances, the ultrafine particles to be purified have a high crystallinity even if they are made into ultrafine particles, and the expected effect of improving the dissolution rate in the solvent and the solubility (or dispersibility) of the supersaturation degree can be obtained. There was nothing.
本発明の目的は、新たな種類の超微粒子を製造する方法
を提供することである。An object of the present invention is to provide a method for producing a new type of ultrafine particles.
本発明の他の目的は、溶媒に対する溶解性・分散性を高
めた非晶質有機物超微粒子を製造する方法を提供するこ
とである。Another object of the present invention is to provide a method for producing amorphous organic material ultrafine particles having improved solubility and dispersibility in a solvent.
反応室内に独立に加熱制御できる主るつぼと補助るつぼ
とを準備し、反応室内に不活性ガス雰囲気を導入し、主
るつぼと補助るつぼとをそれぞれ所定温度に加熱し、超
微粒子を堆積させるための基板を冷却し、目的物質であ
る有機物質を主るつぼから、目的物質の結晶化を妨げる
不純物を補助るつぼから同時に蒸発させ、両者の混合物
を非晶質の超微粒子として前記基板上に堆積させる。Prepare a main crucible and an auxiliary crucible that can be independently heated and controlled in the reaction chamber, introduce an inert gas atmosphere into the reaction chamber, heat the main crucible and the auxiliary crucible to predetermined temperatures, respectively, and deposit the ultrafine particles. The substrate is cooled, and the organic substance, which is the target substance, is simultaneously evaporated from the main crucible and the impurities that hinder the crystallization of the target substance from the crucible, and the mixture of both is deposited as amorphous ultrafine particles on the substrate.
目的物質と添加物とは、初めに各るつぼに装架しても、
少量ずつ貯蔵部から供給してもよい。Even if the target substance and additives are mounted on each crucible first,
You may supply from a storage part little by little.
［作用］ 非晶質超微粒子の製造は、るつぼから超微粒子原料を蒸
発させ、不活性雰囲気ガスと衝突をさせることによって
行われる。結晶化を阻害させるために、結晶化を妨げる
不純物を目的物質に添加するため、目的物質と一緒に結
晶化を妨げる不純物をるつぼに投入すると、るつぼ内で
加熱され蒸発する際に、選択的蒸発が起り、得られる超
微粒子としては不純物濃度が所期のものにならないこと
が多い。[Operation] Amorphous ultrafine particles are produced by evaporating the ultrafine particle raw material from the crucible and colliding it with an inert atmosphere gas. In order to inhibit crystallization, impurities that prevent crystallization are added to the target substance, so if impurities that prevent crystallization are added to the crucible together with the target substance, selective evaporation occurs when the crucible is heated and vaporized. In many cases, the resulting ultrafine particles do not have the desired impurity concentration.
主るつぼと別に独立に加熱制御できる補助るつぼを設
け、主るつぼから目的物質である有機物質を、補助るつ
ぼから結晶化を妨げる不純物を蒸発させることにより、
それぞれの蒸発量を独立に制御することが可能になる。
さらに、目的物質である有機物質と結晶化を妨げる不純
物とを別々の蒸発源から同時に蒸発を行い、冷却した基
板上に超微粒子を捕獲させることにより、溶解性・分散
性に優れた非晶質超微粒子を得ることが可能になる。By providing an auxiliary crucible that can independently control heating separately from the main crucible, by evaporating the organic substance that is the target substance from the main crucible and the impurities that prevent crystallization from the auxiliary crucible,
It is possible to control each evaporation amount independently.
Furthermore, the target substance, an organic substance, and impurities that impede crystallization are simultaneously evaporated from different evaporation sources, and the ultrafine particles are captured on the cooled substrate. It becomes possible to obtain ultrafine particles.
そもそも、非晶質物質を得るための一般的な方法とし
て、 物質を急激に冷却してすばやく造粒する方法、 目的物質に不純物を混入し、結晶成長を抑制する方法 等が有る。目的物質の蒸発と並行して添加物を補助るつ
ぼから蒸発させ混合することはの方法によるものであ
る。このようにして、結晶性を低く抑えた非晶質超微粒
子が得られる。In the first place, as a general method for obtaining an amorphous substance, there are a method of rapidly cooling a substance and granulating it rapidly, a method of mixing impurities into a target substance and suppressing crystal growth. Evaporating the additives from the auxiliary crucible and mixing in parallel with the evaporation of the target substance is by the method of. In this way, amorphous ultrafine particles having low crystallinity are obtained.
非晶質超微粒子は、粒径が小さいことにより優れた溶解
性・分散性を有するのに加え、非晶質であることにより
一層溶解性・分散性が向上することが期待される。The amorphous ultrafine particles have excellent solubility and dispersibility due to their small particle size, and it is expected that the amorphous ultrafine particles have further improved solubility and dispersibility due to being amorphous.
［実施例］ 以下、図面を参照して本発明の実施例を説明する。Embodiments Embodiments of the present invention will be described below with reference to the drawings.
第１図は超微粒子作成装置を示す。FIG. 1 shows an apparatus for producing ultrafine particles.
反応室１は弁７を介して排気系２に接続され、また他の
弁８を介して不活性ガス源３に接続されている。The reaction chamber 1 is connected to the exhaust system 2 via a valve 7, and is connected to the inert gas source 3 via another valve 8.
反応室１は、たとえばステンレス製のベース上にステン
レス製ないしガラス製のベルジャーを載せて構成され
る。排気系２は、たとえばロータリポンプと拡散ポンプ
との組合せ等で構成される。不活性ガス源３はHe,Ar等V
III族ガスないしは、所定の原料に対して不活性と見な
せるN2ガス等の不活性ガスを供給する。The reaction chamber 1 is constructed by mounting a bell jar made of stainless steel or glass on a base made of stainless steel, for example. The exhaust system 2 is composed of, for example, a combination of a rotary pump and a diffusion pump. Inert gas source 3 is V such as He and Ar
A Group III gas or an inert gas such as N 2 gas that can be regarded as inert to a predetermined raw material is supplied.
反応室１内には主るつぼ11、補助るつぼ12が配置されて
いる。それぞれのヒータは独立制御可能な電源に接続さ
れている。A main crucible 11 and an auxiliary crucible 12 are arranged in the reaction chamber 1. Each heater is connected to an independently controllable power source.
るつぼ11、12上方には冷却できる基板５が配置される。
基板５は液体窒素系（図示せず）によって液体窒素温度
近くに冷却できる。A substrate 5 which can be cooled is arranged above the crucibles 11 and 12.
The substrate 5 can be cooled to near the liquid nitrogen temperature by a liquid nitrogen system (not shown).
主るつぼ11、補助るつぼ12は、それぞれたとえばヒータ
を兼ねたW,Mo等の高融点金属の容器、ヒータ上に載せた
石英、アルミナ等の容器、ヒータを埋め込んだ石英、ア
ルミナ等の容器等で構成される。The main crucible 11 and the auxiliary crucible 12 are, for example, a container of a high melting point metal such as W and Mo that also serves as a heater, a container of quartz, alumina or the like placed on the heater, a container of quartz or alumina in which a heater is embedded, or the like. Composed.
以下に超微粒子作成の手順を説明する。The procedure for producing ultrafine particles will be described below.
主るつぼ11に有機化合物等の所望目的物質の原料を所望
量仕込み、補助るつぼ12に所望量の結晶化抑制不純物を
仕込む。基板５を配置し、反応室１を気密に封じる。反
応室１内を高真空（たとえば10-5Torr以上の真空）に排
気し、不活性ガス源３から反応室１内にHe、Ar等の不活
性ガスを導入る。不活性ガスを所定の圧力（たとえば0.
1〜10Torr）に調整し、不活性ガス雰囲気を作成する。
不活性ガス雰囲気はフローさせてもよい。The main crucible 11 is charged with a desired amount of a raw material of a desired target substance such as an organic compound, and the auxiliary crucible 12 is charged with a desired amount of crystallization suppressing impurities. The substrate 5 is placed and the reaction chamber 1 is hermetically sealed. The inside of the reaction chamber 1 is evacuated to a high vacuum (for example, a vacuum of 10 −5 Torr or more), and an inert gas such as He and Ar is introduced from the inert gas source 3 into the reaction chamber 1. Inert gas at a given pressure (e.g. 0.
1 to 10 Torr) and create an inert gas atmosphere.
The inert gas atmosphere may be allowed to flow.
主るつぼ11と補助るつぼ12を加熱し、それぞれの原料の
蒸発温度（あるいは昇華温度）として適当な温度に加熱
して、主るつぼ11から目的物質、補助るつぼ12から結晶
化抑制不純物を同時に蒸発させる。The main crucible 11 and the auxiliary crucible 12 are heated to an appropriate temperature as the evaporation temperature (or sublimation temperature) of each raw material, and the target substance from the main crucible 11 and the crystallization suppressing impurities from the auxiliary crucible 12 are evaporated at the same time. .
同時に蒸発した目的物質の分子（ないし原子）と結晶化
抑制物質の分子（ないし原子）とは、雰囲気ガスの不活
性ガス分子と衝突を繰り返しつつ、冷却、成長・混合
し、混合物の超微粒子となって基板５上に堆積する。超
微粒子は、不活性ガス分子との衝突によって急激に冷却
され、かつ結晶化抑制物質を含んでいるため、非晶質と
なる。また、基板５が冷却されているので成長し、基板
５に衝突した超微粒子はそこで捕獲される。At the same time, the molecules (or atoms) of the target substance and the molecules (or atoms) of the crystallization-inhibiting substance that have evaporated are repeatedly cooled, grown and mixed while repeatedly colliding with the inert gas molecules of the atmosphere gas, and become ultrafine particles of the mixture. Then, it is deposited on the substrate 5. The ultrafine particles are rapidly cooled by the collision with the inert gas molecules, and contain the crystallization suppressing substance, so that they become amorphous. Further, since the substrate 5 is cooled, the ultrafine particles that grow and collide with the substrate 5 are captured there.
たとえば、目的物質は難溶性薬品等の有機物質、結晶化
抑制物質は乳糖、メチルセルロース等である。For example, the target substance is an organic substance such as a poorly soluble drug, and the crystallization-inhibiting substance is lactose or methylcellulose.
真空容器内にHeガスを導入し、真空度を1Torrに調整し
た後、目的物質1gの入った主るつぼと、添加物であるＬ
−ロイシン1gの入った補助るつぼをそれぞれ加熱する。
主るつぼ及び補助るつぼをそれぞれ270℃及び200℃に調
節して蒸発させると、るつぼ上部に設置されたガラス基
板上に、混合超微粒子が付着する。生成された超微粒子
における目的物質と添加物の混合比率は１対１であっ
た。After introducing He gas into the vacuum vessel and adjusting the degree of vacuum to 1 Torr, the main crucible containing 1 g of the target substance and the additive L
Heat each auxiliary crucible containing 1 g of leucine.
When the main crucible and the auxiliary crucible are adjusted to 270 ° C. and 200 ° C. respectively and evaporated, the mixed ultrafine particles adhere to the glass substrate installed on the upper part of the crucible. The mixing ratio of the target substance and the additive in the generated ultrafine particles was 1: 1.
なお、上述の超微粒子製造方法において、加熱方法は抵
抗加熱、ハロゲンランプやレーザ光による光加熱・誘導
加熱等の種々の方法を用いることができる。In addition, in the above-mentioned method for producing ultrafine particles, various heating methods such as resistance heating, light heating using a halogen lamp or laser light, and induction heating can be used.
また、特願平１−85149号で提案したように反応室内に
さらに原料収納部および原料収納部から各るつぼへ原料
を搬送するための搬送具を複数備えてもよい。Further, as proposed in Japanese Patent Application No. 1-85149, the reaction chamber may be further provided with a plurality of raw material storage parts and a plurality of transport tools for transporting the raw materials from the raw material storage parts to the respective crucibles.
原料収納部は、原料を収納し、適宜取り出すことのでき
もので、たとえばステンレス製の棚、開閉できる出口を
底部に持つ容器等で構成される。The raw material storage portion can store the raw material and take it out appropriately, and is composed of, for example, a stainless steel shelf, a container having an openable / closable outlet at the bottom, and the like.
搬送具は、ギヤ等の駆動手段で駆動される匙部材などで
構成される。The carrier is composed of a spoon member driven by a driving unit such as a gear.
このような構成のばあいは、各のるつぼの中には最初は
原料は投入せずに各るつぼを所望温度に加熱できる。With such a configuration, it is possible to heat each crucible to a desired temperature without initially charging the raw material into each crucible.
各るつぼが所定の温度に達した後、原料収納部から少量
ずつ原料を間欠的あるいは連続的にそれぞれのるつぼ内
に投入する。After each crucible reaches a predetermined temperature, a small amount of raw material is intermittently or continuously charged into each crucible from the raw material storage unit.
原料を間欠的ないし連続的に供給する方法としては、 原料収納部とるつぼの間で原料を搬送する役目を担う
匙部材等をプーリやギヤ等を用いて往復運動させる方法
のほか、 ベルトコンベヤを原料収納部からるつぼ上方に設置
し、原料収納部から少量ずつベルトコンベヤに原料を落
とし、るつぼ上に搬送する方法、 原料収納部からるつぼ上へ搬送路を形成し、原料収納
部下部に開口部を設けて原料を振動等によって、少量ず
つ搬送路に投入し、搬送路に沿って原料をるつぼに運ぶ
方法、 これらの組合わせ等 があり、任意に採用できる。As a method of intermittently or continuously supplying the raw material, in addition to a method of reciprocating a spoon member that plays a role of conveying the raw material between the raw material storage section and the crucible using a pulley or a gear, a belt conveyor is used. Installed above the crucible from the raw material storage part, drop the raw material little by little from the raw material storage part onto the belt conveyor and convey it onto the crucible. Form a transfer path from the raw material storage part to the crucible, and open the bottom part of the raw material storage part. There is a method of providing the raw material little by little into the transport path by vibration and the like, and transporting the raw material to the crucible along the transport path, a combination of these, and any method can be adopted.
原料を原料収納部から少量ずつ間欠的あるいは連続的に
るつぼ内に投入すれば、短時間の内に原料を蒸発、気化
させることができる。短時間内に蒸発するので選択的蒸
発によって原料の組成が変化することが少ない。If the raw material is intermittently or continuously put into the crucible from the raw material storage portion little by little, the raw material can be evaporated and vaporized within a short time. Since it evaporates within a short time, the composition of the raw material rarely changes due to selective evaporation.
なお、１つの補助るつぼを用いる場合を説明したが、補
助るつぼの数は複数でもよい。Although the case of using one auxiliary crucible has been described, the number of auxiliary crucibles may be plural.
添加物は、目的物質の用途に不都合を生じない安定な有
機化合物とすればよい。その種類は１つに限らない。The additive may be a stable organic compound that does not cause any inconvenience in the intended use of the target substance. The type is not limited to one.
上に述べたような方法によって、目的物質に不純物とし
て、許容できる量の添加物が混入した超微粒子が作成さ
れる。超微粒子中の目的物質と添加物との組成比は、各
々の蒸発量を独立して制御することでコントロールでき
る。By the method as described above, ultrafine particles in which an acceptable amount of the additive is mixed as an impurity with the target substance is prepared. The composition ratio of the target substance and the additive in the ultrafine particles can be controlled by independently controlling the evaporation amount of each.
［発明の効果］ 以上述べたように、本発明によれば目的物質に所望量の
添加物を混入した超微粒子を製造することができる。[Effects of the Invention] As described above, according to the present invention, it is possible to produce ultrafine particles in which a desired amount of an additive is mixed with a target substance.
結晶化抑制効果を有する不純物を混入することにより、
結晶性を抑制した非晶質性の高い超微粒子が得られる。By mixing impurities that have the effect of suppressing crystallization,
Ultrafine particles with high crystallinity with suppressed crystallinity can be obtained.
非晶質性の超微粒子は、優れた溶解性・分散性を示す。Amorphous ultrafine particles exhibit excellent solubility and dispersibility.
第１図は本発明の実施例に用いる超微粒子製造装置の断
面図、 第２図は従来技術による超微粒子製造装置の断面図であ
る。 図において、 １……反応室 ２……排気系 ３……不活性ガス源 ４……るつぼ 7,8……弁 11……主るつぼ 12……補助るつぼFIG. 1 is a sectional view of an ultrafine particle manufacturing apparatus used in an embodiment of the present invention, and FIG. 2 is a sectional view of an ultrafine particle manufacturing apparatus according to a conventional technique. In the figure, 1 ... Reaction chamber 2 ... Exhaust system 3 ... Inert gas source 4 ... Crucible 7,8 ... Valve 11 ... Main crucible 12 ... Auxiliary crucible
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 昭63−39631（ＪＰ，Ａ) 特開 昭57−165030（ＪＰ，Ａ) 特開 昭63−45362（ＪＰ，Ａ) 実開 昭62−191862（ＪＰ，Ｕ) ─────────────────────────────────────────────────── ─── Continuation of the front page (56) References JP-A-63-39631 (JP, A) JP-A-57-165030 (JP, A) JP-A-63-45362 (JP, A) Actual development Sho-62- 191862 (JP, U)
Claims (1)
と補助るつぼとを準備する工程と、 反応室内に不活性ガス雰囲気を導入し、主るつぼと補助
るつぼとをそれぞれ所定温度に加熱する工程と、 超微粒子を堆積させるための基板を冷却する工程と、 目的物質である有機物質を主るつぼから、目的物質の結
晶化を妨げる不純物を補助るつぼから同時に蒸発させ、
両者の混合物を非晶質の超微粒子として前記基板上に堆
積させる工程とを含む超微粒子の製造方法。1. A step of preparing a main crucible and an auxiliary crucible capable of independently controlling heating in the reaction chamber, and a step of introducing an inert gas atmosphere into the reaction chamber and heating the main crucible and the auxiliary crucible to respective predetermined temperatures. And a step of cooling the substrate for depositing the ultrafine particles, and simultaneously evaporating the organic substance, which is the target substance, from the main crucible and the impurities that hinder the crystallization of the target substance from the crucible,
And a step of depositing a mixture of the both as amorphous ultrafine particles on the substrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1225059A JPH0753236B2 (en) | 1989-08-31 | 1989-08-31 | Ultrafine particle manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1225059A JPH0753236B2 (en) | 1989-08-31 | 1989-08-31 | Ultrafine particle manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0389938A JPH0389938A (en) | 1991-04-15 |
| JPH0753236B2 true JPH0753236B2 (en) | 1995-06-07 |
Family
ID=16823397
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1225059A Expired - Fee Related JPH0753236B2 (en) | 1989-08-31 | 1989-08-31 | Ultrafine particle manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0753236B2 (en) |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57165030A (en) * | 1981-04-06 | 1982-10-09 | Hitachi Ltd | Preparation of ultrafine particle |
| JPS62191862U (en) * | 1986-05-27 | 1987-12-05 | ||
| JPH0683780B2 (en) * | 1986-08-05 | 1994-10-26 | 新技術事業団 | Method for producing organic fine particles |
| JPS6345362A (en) * | 1986-08-11 | 1988-02-26 | Matsushita Electric Ind Co Ltd | Method for producing phthalocyanine compound thin film |
-
1989
- 1989-08-31 JP JP1225059A patent/JPH0753236B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0389938A (en) | 1991-04-15 |
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