JPS58136701A - Method and apparatus for treating surface of fine particle - Google Patents
Method and apparatus for treating surface of fine particleInfo
- Publication number
- JPS58136701A JPS58136701A JP57017577A JP1757782A JPS58136701A JP S58136701 A JPS58136701 A JP S58136701A JP 57017577 A JP57017577 A JP 57017577A JP 1757782 A JP1757782 A JP 1757782A JP S58136701 A JPS58136701 A JP S58136701A
- Authority
- JP
- Japan
- Prior art keywords
- fine particles
- plasma
- container
- particles
- treatment
- 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.)
- Granted
Links
- 239000010419 fine particle Substances 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims description 16
- 239000002245 particle Substances 0.000 claims abstract description 24
- 238000005096 rolling process Methods 0.000 claims abstract description 7
- 238000004381 surface treatment Methods 0.000 claims description 24
- 238000000576 coating method Methods 0.000 claims description 7
- 238000011282 treatment Methods 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000005530 etching Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000012986 modification Methods 0.000 claims description 4
- 230000004048 modification Effects 0.000 claims description 4
- 238000009832 plasma treatment Methods 0.000 claims 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 27
- 239000007789 gas Substances 0.000 description 27
- 229910052759 nickel Inorganic materials 0.000 description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 239000007788 liquid Substances 0.000 description 8
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 6
- 239000005977 Ethylene Substances 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 4
- 238000001941 electron spectroscopy Methods 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 229920006254 polymer film Polymers 0.000 description 4
- 239000011521 glass Substances 0.000 description 3
- 229910000480 nickel oxide Inorganic materials 0.000 description 3
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910001868 water Inorganic materials 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- WMIYKQLTONQJES-UHFFFAOYSA-N hexafluoroethane Chemical compound FC(F)(F)C(F)(F)F WMIYKQLTONQJES-UHFFFAOYSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 150000001282 organosilanes Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
Abstract
Description
【発明の詳細な説明】
本発明は微粒子の表面処理方法及びその装置に関するも
のである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for surface treatment of fine particles and an apparatus therefor.
一般に微粒子は種々の用途に用いられており、例えば鉄
の微粒子は記録用磁気テープの磁性材料として広く用い
られているが、この鉄の微粒子は通常空気雰囲下にて保
存されており、このため表面が酸化されてかなり厚い酸
化膜が形成されている。従って鉄の微粒子による記録用
磁気テープの製造においては酸化膜のない鉄の微粒子を
グラスチック等より成るベースチーブに塗布することが
必要とされることから、この微粒子をベースチーブに塗
布する前に当該微粒子に表面の酸化膜を除去するための
表面処理を施すことが必要とされる。Generally, fine particles are used for various purposes. For example, fine iron particles are widely used as magnetic materials for recording magnetic tapes, but these fine particles are usually stored in an air atmosphere. Therefore, the surface is oxidized and a fairly thick oxide film is formed. Therefore, in the production of recording magnetic tapes using fine iron particles, it is necessary to apply fine iron particles without an oxide film to a base plate made of glass or the like, so before applying these fine particles to the base plate, It is necessary to perform surface treatment to remove the oxide film on the surface.
そして表面処理後の、酸化膜が除去された鉄の微（３）
粒子は酸素にふれないようにしてベーステープに塗布さ
れた上やはり酸素にふれないようにして樹脂等により被
覆して記録用磁気１−グが形成される。筐たこの他にも
微粒子にコーティング、前面改質等の表面処理を施すこ
とが広くイ１″なわｒじＣいる。After surface treatment, the iron particles (3) from which the oxide film has been removed are coated on a base tape so as not to come into contact with oxygen, and then coated with a resin or the like so as not to come into contact with oxygen for recording purposes. A magnetic 1-group is formed. In addition to coatings, surface treatments such as coating and front surface modification are widely applied to fine particles.
従来このような微粒子の表面処理方法とし、ては、液体
或いはペースト状の物質を用いる方法が広く行なわれて
いる１つこれは、例えば酸化膜をエツチングするために
は微粒子をアルカリ性水溶液中を通過せしめて酸化膜を
溶解除去する方法、微粒子をコーディングするためには
、微粒子を有機溶液中を通過せしめて表向に樹脂被膜を
形成する方法等である。Conventionally, one of the widely used methods for surface treatment of such fine particles is to use a liquid or paste-like substance.For example, in order to etch an oxide film, fine particles are passed through an alkaline aqueous solution. At least the oxide film is dissolved and removed, and in order to coat the fine particles, the fine particles are passed through an organic solution to form a resin coating on the surface.
しかしながらこのように液体或いはペースト状の物質を
用いる方法においては、通常装置が複雑となり、又２種
類以上の液体を用いて段階的に表冒１
面処理を行なう必要がある場合には、一つの油体から次
の液体へ順次微粒子を入れなければならないか、その際
酸素にふれさせずに微粒子を移動させるのは極めて困難
であり、酸化防止の必要かめる場合には極めて不利であ
る。捷たこの場合には各液体が混入するおそれがあり、
溶液の使用寿命或いは作用が低下することともなる。ま
た使用済の不要になった液体を廃棄する場合、公害防止
上の観点から相当に安全性の高い処理を施した上廃棄す
ることが要請きれコスト高になる。However, in methods using liquid or paste-like substances, the equipment is usually complicated, and when it is necessary to perform surface treatment in stages using two or more types of liquids, one It is extremely difficult to transfer the fine particles from one oil body to the next liquid without exposing them to oxygen, which is extremely disadvantageous in cases where oxidation prevention is required. In this case, there is a risk that various liquids may be mixed in.
The service life or effectiveness of the solution may also be reduced. Furthermore, when disposing of used liquid that is no longer needed, it is required to perform extremely safe treatment from the viewpoint of pollution prevention before disposal, which increases costs.
本発明者らは、以−ヒのような事情に基き鋭意研究を重
ねた結果、高真空中で微粒子をプラズマ処理することに
よりエツチング、コーティング、表面改質等の各種の表
面処理を容易に達成でき、液体を用いる方法における上
述の欠点を解消することができることを見い出し本発明
を完成するに至った。As a result of intensive research based on the above circumstances, the present inventors have found that various surface treatments such as etching, coating, and surface modification can be easily achieved by plasma treating fine particles in a high vacuum. The present invention has been completed based on the discovery that the above-mentioned drawbacks of the method using a liquid can be overcome.
本発明の目的は、プラズマの作用により微粒子の表面処
理を均一に行なうことができる微粒子の表面処理方法を
提供することにある。SUMMARY OF THE INVENTION An object of the present invention is to provide a method for surface treatment of fine particles, which enables uniform surface treatment of fine particles by the action of plasma.
本発明の他の１的は、プラズマの作用により微粒子の表
面処理を均一に行なうことができる微粒子の表面処理装
置を提供することにある。Another object of the present invention is to provide a surface treatment device for fine particles that can uniformly treat the surface of fine particles by the action of plasma.
（５）
本発明方法の特徴とするところは、プラズマが発生して
いる空間内において、微粒子を転動させ、更に空間を落
下せしめることにより当該微粒子の表面をプラズマ処理
する点にある。(5) The method of the present invention is characterized in that the surfaces of the particles are treated with plasma by rolling the particles in a space where plasma is generated and then causing them to fall through the space.
本発明装置の特徴とするところは、微粒子が収納される
回動自在な容器と、この容器内にプラズマを形成するプ
ラズマ発生機構とを有する点にある。The device of the present invention is characterized by having a rotatable container in which fine particles are stored, and a plasma generation mechanism that forms plasma within the container.
以下本発明を具体的に説明する。The present invention will be specifically explained below.
本発明方法においては、プラズマが発生している空間内
において、処理すべき微粒子を転動させながら上昇落下
せしめ、これに前記プラズマを作用せしめて当該微粒子
の表面をプラズマ処理する。In the method of the present invention, fine particles to be treated are made to rise and fall while rolling in a space where plasma is generated, and the plasma is applied to the fine particles to plasma-treat the surfaces of the fine particles.
斯かる方法によれば、表面処理にプラズマを用いるため
、前述の液体を用いる方法における欠点を除去すること
ができる上、処理すべき微粒子をプラズマ中を転動させ
ながら上昇落下せしめるため、微粒子の表面処理を表面
全体に亘って均一に行なうことができる。According to this method, since plasma is used for surface treatment, the drawbacks of the above-mentioned method using a liquid can be eliminated, and the fine particles to be treated are caused to rise and fall while rolling in the plasma, so that the fine particles can be treated easily. Surface treatment can be performed uniformly over the entire surface.
本発明装置においては、例えば第１図に示すよ（６）
うに、例えばガラス等より成る絶縁性の両端開口の円筒
３の当該両端開口をそれぞれ塞ぐよう電極板ＩＡ 、Ｉ
Ｂを兼ねる一対の金属製の側板２Ａ 。In the device of the present invention, as shown in FIG. 1 (6), for example, electrode plates IA and I are used to close the openings at both ends of an insulating cylinder 3 made of glass or the like and having openings at both ends.
A pair of metal side plates 2A that also serve as B.
２Ｂを配設して容器４を形成し、前記円筒３の例えば中
心軸Ｘ上に沿って前記側板２Ａ 、２Ｂをそれぞれ貫通
してこれより外方に伸びるガラス等より成る絶縁性の回
動軸５を当該側板２Ａ 、２Ｂに固定して設け、この回
動軸５の両端をこれが水平に位置するよう、真空槽８内
に設けた支持枠７Ａ。2B to form a container 4, and an insulating pivot shaft made of glass or the like that extends outward from the side plates 2A and 2B by passing through the side plates 2A and 2B, for example, along the central axis X of the cylinder 3. 5 is fixed to the side plates 2A and 2B, and the support frame 7A is provided in the vacuum chamber 8 so that both ends of the rotation shaft 5 are positioned horizontally.
７Ｂにより回動自在に支持せしめて前記容器４を真空槽
８内に配設し、前記回動軸５の一端にはギア等を介して
モーター６を接続し、側板２Ａ、２Ｂには複数の透孔９
を設けて、例えばその一方の側板２Ａの透孔９に接近対
向し得るようその供給口１０を近接して位置せし２めた
、プラズマ形成用ガスを供給するガス供給管１１を設け
ると共に、真空槽８の例えば下底壁８１に排気管１２を
接続して設け、そして側板２Ａ 、２Ｂ を兼ねる電
極板ＩＡ 、ＩＢを含み、この電極板ＩＡ 、 ｌｆｌ
の各々にブラシ先端が接触するよう真空槽８に対して固
（７）
定して設けた電極ブラシ１４Ａ 、 １４Ｂと、この電
極ブラシ１４Ａ 、 １４Ｂに接続した電源１３とによ
りプラズマ発生機構１５を構成する。The container 4 is rotatably supported by 7B and placed in a vacuum chamber 8. A motor 6 is connected to one end of the rotation shaft 5 via a gear or the like, and a plurality of Through hole 9
and a gas supply pipe 11 for supplying plasma forming gas, the supply port 10 of which is located close to the through hole 9 of one of the side plates 2A, for example, is provided, An exhaust pipe 12 is connected to, for example, a lower bottom wall 81 of the vacuum chamber 8, and includes electrode plates IA and IB that also serve as side plates 2A and 2B, and these electrode plates IA and lfl.
A plasma generation mechanism 15 is constituted by electrode brushes 14A, 14B fixedly fixed (7) to the vacuum chamber 8 so that the tips of the brushes are in contact with each of the electrode brushes 14A, 14B, and a power source 13 connected to the electrode brushes 14A, 14B. do.
本発明方法においては、以上のような構成の装置を用い
例えば次のようにして微粒子の表面処理を行なう。即ち
、直径数＋Ａ〜数十数十機粒子から成る集合体を容器４
内に収納し、真空槽８内を例えば真空ポンプ（図示せず
）等により排気して高真空状態とした上でガス供給管１
１よりプラズマ形成用ガスを供給して容器４内に導入す
ると共に、電源１３より電極ブラシ１４Ａ 、 １４Ｂ
を介し７て電極板ＩＡ 、 ｌｆ３に電力を供給して容
器４内にプラズマ形成用ガスのプラズマを形成し、更に
モーター６を駆動せしめて容器４を例えば５Ｑ ｒ、
ｐ、 ｍ。In the method of the present invention, the surface treatment of fine particles is performed, for example, in the following manner using the apparatus configured as described above. That is, an aggregate consisting of particles with a diameter of several + A to several dozen particles is placed in a container 4.
After evacuating the inside of the vacuum chamber 8 using a vacuum pump (not shown) or the like to create a high vacuum state, the gas supply pipe 1 is
1 supplies a plasma forming gas and introduces it into the container 4, and a power source 13 supplies electrode brushes 14A and 14B.
Electric power is supplied to the electrode plates IA and lf3 via 7 to form a plasma of plasma forming gas in the container 4, and the motor 6 is further driven to move the container 4 to, for example, 5Qr,
p, m.
以上好ましくは２０Ｏｒ、 ｐ、 ｍ、以上の回転速度
で回転させながら、容器４内の微粒子に前記プラズマ形
成用ガスのプラズマを作用せしめ、以って微粒子の表面
処理を行なう。The plasma of the plasma forming gas is applied to the particles in the container 4 while rotating at a rotational speed of preferably 20 Or, p, m or more, thereby surface-treating the particles.
プラズマ形成用ガスとしては、微粒子の表面をコーディ
ングする場合には例えばハイドロカーボン、フルオロカ
ーボン、シラン、オルガノシラン、オルガノメタル等の
微粒子の表面にプラズマ重合膜を形成するものであれば
よく、微粒子の表面を改質する場合例えば水に対する濡
れを良くする場合には酸素、窒素、−酸化炭素、或いは
これらの混合ガスを用いることができ、微粒子の表面を
エンチングする場合、例えば微粒子が金属或いは酸化物
である場合にはパーフルオロメタン、パーフルオロエタ
ン、フッ索ガス等ハロゲンヲ含ｔｒ化合物ガスを用いる
ことができ、微粒子が有機物である場合には酸素を用い
ることができる。When coating the surface of fine particles, the plasma forming gas may be any gas that forms a plasma polymerized film on the surface of the fine particles, such as hydrocarbon, fluorocarbon, silane, organosilane, organometal, etc. For example, to improve wettability with water, oxygen, nitrogen, carbon oxide, or a mixture of these gases can be used, and to etch the surface of fine particles, for example, if the fine particles are made of metal or oxide. In some cases, a halogen-containing compound gas such as perfluoromethane, perfluoroethane, or fluorine gas can be used, and if the fine particles are organic, oxygen can be used.
このような方法によれば、容器４を回転せしめるため、
容器４内の微粒子は当該容器４の回転に応じてプラズマ
形成用ガスの７−ラズマ中において転動しながら上昇し
、そして更に自重で落下するようになり、しかもこの上
昇・落下が繰り返さ沃このだめ当該微粒子がその表面全
体に亘り均一にプラズマの作用を受けるようになり、こ
の結果当該微粒子の表面が均一にプラズマ処理される。According to such a method, in order to rotate the container 4,
As the container 4 rotates, the fine particles in the container 4 rise while rolling in the plasma forming gas plasma, and then fall down due to their own weight, and this rising and falling is repeated. Instead, the entire surface of the fine particles is uniformly affected by the plasma, and as a result, the surface of the fine particles is uniformly plasma-treated.
また第１図に示した装置によれば、大量の微粒子を（９
）
同時に均一な表面処理をすることができ工業上極めて有
利である上、プラズマ形成用ガスを適宜取り替えてプラ
ズマ条件を変えることにより同一の装置で、エツチング
処理、コーティング処理、表面改質処理等の種々の表面
処理を容易に行なうことができ極めて便利である。Furthermore, according to the apparatus shown in Fig. 1, a large amount of fine particles (9
) It is possible to perform uniform surface treatment at the same time, which is extremely advantageous industrially, and by changing the plasma conditions by appropriately replacing the plasma forming gas, it is possible to perform etching treatment, coating treatment, surface modification treatment, etc. with the same equipment. It is extremely convenient as various surface treatments can be easily performed.
以上において第２図 （イ）及び（ロ）に不すように容
器４を構成する円筒３０内壁３１に当該円筒３の軸と平
行に伸びる複数（図示の例では８個）の細長い板状の攪
拌部材３２を当該円筒３の内方に突出するよう設けてお
けば、容器４が回転したときに微粒子をこの攪拌部材３
２により確実に上昇・落下せしめることができ微粒子の
表面処理を均一に行なうことがさらに一層確実なものと
なる。In the above, as shown in FIGS. 2(A) and 2(B), on the inner wall 31 of the cylinder 30 constituting the container 4, there are a plurality of (eight in the illustrated example) elongated plate-shaped plates extending parallel to the axis of the cylinder 3. If the stirring member 32 is provided so as to protrude inward from the cylinder 3, when the container 4 rotates, the fine particles will be transferred to the stirring member 3.
2, it is possible to raise and fall the particles reliably, thereby further ensuring uniform surface treatment of the particles.
ここで攪拌部材３２の伸びる方向は円筒３の軸に対して
若干斜めであってもよい。なお攪拌部材３２は円筒３と
一体に形成してもよい１−１円筒３とは別な部材で形成
してもよい。Here, the direction in which the stirring member 32 extends may be slightly oblique to the axis of the cylinder 3. Note that the stirring member 32 may be formed integrally with the cylinder 3 or may be formed of a separate member from the 1-1 cylinder 3.
第１図に示した装置においては容器４を回転せしめる構
成としたが、微粒子をプラズマ中で転勤（１０）
せしめる手段としては、斯かる例に限らず例えば容器４
を全回転運動させるのではなく回動軸５を中心に振子の
ような揺動運動せしめるようギア等を構成してもよい。Although the apparatus shown in FIG. 1 has a configuration in which the container 4 is rotated, the means for causing the fine particles to be transferred (10) in the plasma is not limited to this example.
A gear or the like may be configured so as to cause the rotation axis 5 to oscillate like a pendulum around the rotation axis 5 instead of making a full rotational movement.
また容器４の形状は角筒型でもよい。Further, the shape of the container 4 may be a rectangular tube type.
前記プラズマ発生機構１５における電源１３としては、
直流電源、オーディオ周波数電源、高周波電源等を用い
ることができる。The power source 13 in the plasma generation mechanism 15 includes:
A DC power source, an audio frequency power source, a high frequency power source, etc. can be used.
前記プラズマ発生機構１５は既述の例に限らず、例えば
第３図に示すように長尺な円筒型容器４２の外周にコイ
ル１８を巻回せしめてこのコイル１８に高周波電源１３
１を接続した構成、或いは円筒型容器４２の外周に設け
たはしご状のマイクロ波導波路材を介してマイクロ波電
源によりマイクロ波エネルギーを加えるようにした構成
等、微粒子が収納される容器内にプラズマが形成される
構成であればよい。The plasma generation mechanism 15 is not limited to the example described above, but for example, as shown in FIG.
1 is connected, or a configuration in which microwave energy is applied by a microwave power source via a ladder-shaped microwave waveguide material provided on the outer periphery of the cylindrical container 42. Any configuration is sufficient as long as it forms.
以下本発明の実施例について説明する。Examples of the present invention will be described below.
実施例１
第１図に７トシた構成の装置を用い、平均粒径（１１）
ｌｏｏｏＸ−のニッケル微粒子を容器４内に収納Ｌ、真
空槽８内を排気して５０ミリＴｏｒｒ の真空状態と
なるようガス供給管１１よりプラズマ形成用ガスとして
エチレンガスを流量５０ ＴＩｔ／分の割合で供給して
これを容器４内に導入すると共に電源１３より電極板Ｉ
Ａ 、ＩＢに２０ Ｗの電力を供給して容器４内にエチ
レンガスのプラズマを形成しながら、モーター６を駆動
せしめて容器４を例えば１５０ ｒ、ｐ、ｍ、の回転速
度で回転させ、約２時間に亘りプラズマを作用させてニ
ッケル微粒子の表面処理を行ない、以−ってニッケル微
粒子の表面がエチレンガスのプラズマによる重合膜で被
覆された被覆微粒子を得た。Example 1 Using an apparatus having the same configuration as shown in FIG. 1, fine nickel particles with an average particle size (11) loooX- were stored in a container 4, and the vacuum chamber 8 was evacuated to create a vacuum of 50 mmTorr. Ethylene gas is supplied from the gas supply pipe 11 as a plasma forming gas at a flow rate of 50 TIt/min, and is introduced into the container 4, and the electrode plate I is supplied from the power supply 13.
A, while supplying 20 W of power to the IB to form an ethylene gas plasma in the container 4, drive the motor 6 to rotate the container 4 at a rotational speed of, for example, 150 r, p, m. The surface of the nickel fine particles was treated by applying plasma for two hours, thereby obtaining coated fine particles in which the surface of the nickel fine particles was coated with a polymer film formed by ethylene gas plasma.
得られた被覆微粒子をＥＳＣＡ（電子分光法）により調
べたところニッケルの２Ｐ丁 ピークが現われず当該被
覆微粒子の表面に浮さ数十Ｎ以上のエチレンガスのプラ
ズマによる重合膜が形成されていることが確認された。When the obtained coated fine particles were examined by ESCA (electron spectroscopy), no 2P peak of nickel appeared, indicating that a polymer film was formed by plasma of ethylene gas floating on the surface of the coated fine particles at tens of N or more. was confirmed.
次に得られた被覆微粒子を水中に分散させ、この中から
一滴とりだしこれを銅メツシーに厚さ５００にのコロジ
オン膜を張った基板上に滴下した後乾燥させ、透過型電
子顕微鏡で観察したところ被覆微粒子表面の１鎚の厚さ
は表面全体に亘って４０士５大の範囲内であり極めて均
一性の高いものであった。Next, the obtained coated fine particles were dispersed in water, one drop was taken out, and this was dropped onto a substrate made of copper mesh coated with a 500 mm thick collodion film, dried, and observed with a transmission electron microscope. The thickness of the surface of the coated fine particles was within the range of 40 to 5 over the entire surface, and was highly uniform.
実施例２
第１図に示した構成の装置を用い、平均粒径１０００＾
の表面が酸化されたニッケル微粒子を容器４内に収納し
、真空槽８内を排気して３０ミリＴｏｒｒ の真空状態
となるようガス供給管ｌｌよりプラズマ形成用ガスとし
てアルゴンガスを流量５０ゴ／分の割合で供給してこれ
を容器４内に導入すると共に電源１３より電極板ＩＡ
、 ｌｆｌに１５０ Ｗの電力を供給して容器４内にア
ルゴンガスのプラズマを形成しながら、モーター６を駆
動せしめて容器４を例えば１５０ ｒ、 ｐ、 ｍ、
の回転速度で回転させ、約３０分間に亘りプラズマを作
用させてニッケル微粒子の表面処理を行ない、以ってニ
ッケル微粒子の表面がエツチングされて酸化膜が除去さ
れた純ニツケル微粒子を得た。Example 2 Using a device with the configuration shown in Figure 1, an average particle size of 1000^
Fine nickel particles with oxidized surfaces are stored in a container 4, and argon gas is supplied as a plasma forming gas from a gas supply pipe 11 at a flow rate of 50 mTorr to create a vacuum state of 30 mTorr by evacuating the inside of the vacuum chamber 8. The electrode plate IA is supplied from the power source 13 at the same time as it is introduced into the container 4.
, while supplying 150 W of power to lfl to form an argon gas plasma in the container 4, drive the motor 6 to move the container 4 to, for example, 150 r, p, m,
The surface of the nickel fine particles was treated by rotating the plate at a rotational speed of 100 mL and applying plasma for about 30 minutes, thereby etching the surface of the nickel fine particles and removing the oxide film to obtain pure nickel fine particles.
（１３）
そして得られた純ニツケル微粒子に実施例１と同様にし
て表面処理を行ない、以って純ニッケル微粒子の表面が
エチレンガスのプラズマによる重合膜で被覆された被覆
微粒子を得た。(13) The obtained pure nickel fine particles were then subjected to surface treatment in the same manner as in Example 1, thereby obtaining coated fine particles in which the surfaces of the pure nickel fine particles were coated with a polymer film formed by ethylene gas plasma.
この被＆微粒千をＥＳＣＡ （電子分光法）により調
べたところ、ニッケルの２Ｐ２ ピークは現われなか
った。次いでこの被覆微粒子をアルゴンイオンビームで
約６秒間エツチングした後再びＥＳＣ：Ａ（電子分光法
）により調べたところ、酸化ニッケルの２Ｐ２ビークは
現われなかった。さらに６秒間同様のエツチングを行な
った後調べたところ酸化ニッケルの２Ｐ２ ピークは
現われなかった。When the 2P2 peak of nickel was examined by ESCA (electron spectroscopy), no 2P2 peak of nickel appeared. Next, the coated fine particles were etched with an argon ion beam for about 6 seconds and then examined again by ESC:A (electron spectroscopy), and no 2P2 peak of nickel oxide appeared. After performing similar etching for another 6 seconds, the 2P2 peak of nickel oxide did not appear.
次に同様のエツチングを６秒間に亘り行なった後Ｈ８Ｃ
Ａ（電子分光法）によりｉｉ＆ｌｉべたところ金属ニッ
ケルの２Ｐ２ ピークが現われ、酸化ニッケルの２Ｐ
（ピークは現われなかった。これよりこの実施例で得ら
れた被覆微粒子は酸化膜がアルゴンガスのプラズマの作
用により確実にエツチングされ、純ニツケル微粒子の表
面がエチレンガスのプラズマによる重合膜で被覆されて
いることがわかった。Next, after performing similar etching for 6 seconds, H8C
A (electron spectroscopy) shows that the 2P2 peak of metallic nickel appears in the ii&li area, and the 2P2 peak of nickel oxide appears.
(No peak appeared. From this, it can be seen that the oxide film of the coated fine particles obtained in this example was reliably etched by the action of argon gas plasma, and the surface of the pure nickel fine particles was coated with a polymer film caused by ethylene gas plasma.) I found out that
（１４）(14)
第１図は不発明徴粒子の表面処理装置の一例を示す説明
用断面図、第２図（イ）及び（ロ）はそれぞれ本発明装
置における容器の一例を示す説明用縦断正面図及び説明
用縦断側面図、第３図は本発明に係る装置におけるプラ
ズマ発生機構の他の例を示す説明図である。
ＩＡ、１Ｂ・・・電極板 ２Ａ、２Ｂ・・・側板３・
・・円筒 ４・・・容器５・・・回動軸
６・・・モーター７Ａ 、 ７Ｂ・・・支持枠
８・・・真空槽８１・・・下底壁 ９・・・透孔
ｌｌ・・ガス供給管 １２・・・排気管１３・・・電
源 １４Ａ、１４Ｂ ・・・電極ブラシ１５・
・・プラズマ発生機構
１８・・・コイル ３２・・・攪拌部材４２・・
・容器
１３１ ・・・高周波電源
代理人 弁理士 大 井 正 彦
第３０
１３１
５−FIG. 1 is an explanatory sectional view showing an example of a surface treatment device for non-inventive particles, and FIGS. 2 (a) and (b) are an explanatory longitudinal sectional front view and an explanatory front view showing an example of a container in the inventive device, respectively. A longitudinal side view and FIG. 3 are explanatory diagrams showing another example of the plasma generation mechanism in the apparatus according to the present invention. IA, 1B... Electrode plate 2A, 2B... Side plate 3.
...Cylinder 4...Container 5...Rotation axis
6...Motor 7A, 7B...Support frame
8... Vacuum chamber 81... Lower bottom wall 9... Through hole 11... Gas supply pipe 12... Exhaust pipe 13... Power supply 14A, 14B... Electrode brush 15...
...Plasma generation mechanism 18...Coil 32...Stirring member 42...
・Container 131 ... High frequency power supply agent Patent attorney Masahiko Oi No. 30 131 5-
Claims (1)
転動させ、更に空間を落下せしめることにより当該微粒
子の表面をプラズマ処理することを％徴とする微粒子の
表面処理方法。 ２）前記プラズマ処理がエツチング処理である特許請求
の範囲第１項記載の微粒子の表面処理方法。 ３）前記プラズマ処理がコーティング処理である特許請
求の範囲第１項記載の微粒子の表面処理方法。 ４）前記プラズマ処理が表面改質処理である特許請求の
範囲第１項記載の微粒子の表面処理方法。 ５）微粒子が収納される回動自在な容器と、この容器内
にプラズマを形成するプラズマ発生機構とを有すること
を特徴°とする微粒子の表（２） 面処理装置。 ６）前記容器の内壁に、容器の回動軸に沿って伸びる攪
拌部材を設けたことを特徴とする特許請求の範囲第５項
記載の微粒子の表面処理装置。[Scope of Claims] 1) A method for surface treatment of fine particles, which includes plasma-treating the surface of fine particles by rolling the fine particles in a space where plasma is generated and then causing the particles to fall through the space. . 2) The method for surface treatment of fine particles according to claim 1, wherein the plasma treatment is an etching treatment. 3) The method for surface treatment of fine particles according to claim 1, wherein the plasma treatment is a coating treatment. 4) The method for surface treatment of fine particles according to claim 1, wherein the plasma treatment is a surface modification treatment. 5) A surface treatment device for fine particles, characterized by comprising a rotatable container in which fine particles are stored, and a plasma generation mechanism for forming plasma in the container. 6) The particle surface treatment apparatus according to claim 5, further comprising a stirring member provided on the inner wall of the container and extending along the rotational axis of the container.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57017577A JPS58136701A (en) | 1982-02-08 | 1982-02-08 | Method and apparatus for treating surface of fine particle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57017577A JPS58136701A (en) | 1982-02-08 | 1982-02-08 | Method and apparatus for treating surface of fine particle |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS58136701A true JPS58136701A (en) | 1983-08-13 |
| JPH024642B2 JPH024642B2 (en) | 1990-01-30 |
Family
ID=11947760
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP57017577A Granted JPS58136701A (en) | 1982-02-08 | 1982-02-08 | Method and apparatus for treating surface of fine particle |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS58136701A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0192373A (en) * | 1987-09-30 | 1989-04-11 | Ishikawajima Harima Heavy Ind Co Ltd | Formation of thin carbon film on raw material having large specific surface by cvd |
| JP2002060943A (en) * | 2000-08-22 | 2002-02-28 | Tohoku Electric Power Co Inc | Method and device for coating high purity silicon |
| JP2008169421A (en) * | 2007-01-10 | 2008-07-24 | Tsubaki Emerson Co | Dlc film deposition system |
| JP2009256804A (en) * | 2009-08-03 | 2009-11-05 | Utec:Kk | Fine particle |
| JP2017075391A (en) * | 2015-08-31 | 2017-04-20 | ウルトラテック インク | Plasma-promoted atomic layer deposition system having rotation reaction tube |
| EP3484810A4 (en) * | 2016-07-15 | 2020-03-25 | Oned Material LLC | Manufacturing apparatus and method for making silicon nanowires on carbon based powders for use in batteries |
| JP2020084222A (en) * | 2018-11-16 | 2020-06-04 | 日本化学工業株式会社 | Method for manufacturing coated particle |
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| JPS5645962A (en) * | 1979-09-25 | 1981-04-25 | Nippon Tokushu Toryo Kk | Asphaltic coating-type vibration-damping material |
| JPS57166373A (en) * | 1981-04-02 | 1982-10-13 | Sumitomo Electric Industries | Manufacture of non-oxide ceramics |
| JPS5822302A (en) * | 1981-07-30 | 1983-02-09 | Nippon Steel Corp | Method of activating treatment of hydrogen-occluded metal |
| JPS5881971A (en) * | 1981-11-11 | 1983-05-17 | Matsushita Electric Ind Co Ltd | Apparatus for depositing film |
| JPS58100601A (en) * | 1981-12-09 | 1983-06-15 | Japan Synthetic Rubber Co Ltd | Coated ultrafine particle or its film and method and device for forming said particle or film |
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| JPS5236759A (en) * | 1975-09-18 | 1977-03-22 | Oki Electric Ind Co Ltd | Method of fixing parts on printed circuit board |
| JPS5641375A (en) * | 1979-09-13 | 1981-04-18 | Matsushita Electric Ind Co Ltd | Sputtering apparatus |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0192373A (en) * | 1987-09-30 | 1989-04-11 | Ishikawajima Harima Heavy Ind Co Ltd | Formation of thin carbon film on raw material having large specific surface by cvd |
| JP2002060943A (en) * | 2000-08-22 | 2002-02-28 | Tohoku Electric Power Co Inc | Method and device for coating high purity silicon |
| JP2008169421A (en) * | 2007-01-10 | 2008-07-24 | Tsubaki Emerson Co | Dlc film deposition system |
| JP2009256804A (en) * | 2009-08-03 | 2009-11-05 | Utec:Kk | Fine particle |
| JP2017075391A (en) * | 2015-08-31 | 2017-04-20 | ウルトラテック インク | Plasma-promoted atomic layer deposition system having rotation reaction tube |
| EP3484810A4 (en) * | 2016-07-15 | 2020-03-25 | Oned Material LLC | Manufacturing apparatus and method for making silicon nanowires on carbon based powders for use in batteries |
| US10862114B2 (en) | 2016-07-15 | 2020-12-08 | Oned Material Llc | Manufacturing apparatus and method for making silicon nanowires on carbon based powders for use in batteries |
| EP3778471A1 (en) * | 2016-07-15 | 2021-02-17 | OneD Material, Inc. | Manufacturing method for making silicon nanowires on carbon based powders for use in batteries |
| US11728477B2 (en) | 2016-07-15 | 2023-08-15 | Oned Material, Inc. | Manufacturing apparatus and method for making silicon nanowires on carbon based powders for use in batteries |
| EP4273296A1 (en) * | 2016-07-15 | 2023-11-08 | OneD Material, Inc. | Manufacturing apparatus and method for making silicon nanowires on carbon based powders for use in batteries |
| EP4292702A3 (en) * | 2016-07-15 | 2024-04-17 | OneD Material, Inc. | Manufacturing apparatus and method for making silicon nanowires on carbon based powders for use in batteries |
| JP2020084222A (en) * | 2018-11-16 | 2020-06-04 | 日本化学工業株式会社 | Method for manufacturing coated particle |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH024642B2 (en) | 1990-01-30 |
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