JP2003342744A - Method for coating powder - Google Patents
Method for coating powderInfo
- Publication number
- JP2003342744A JP2003342744A JP2003075202A JP2003075202A JP2003342744A JP 2003342744 A JP2003342744 A JP 2003342744A JP 2003075202 A JP2003075202 A JP 2003075202A JP 2003075202 A JP2003075202 A JP 2003075202A JP 2003342744 A JP2003342744 A JP 2003342744A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- gas
- coating
- coating liquid
- coating layer
- 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
- 239000000843 powder Substances 0.000 title claims abstract description 150
- 238000000576 coating method Methods 0.000 title claims abstract description 58
- 239000011248 coating agent Substances 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000011247 coating layer Substances 0.000 claims abstract description 38
- 238000003756 stirring Methods 0.000 claims description 52
- 239000007788 liquid Substances 0.000 claims description 45
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 24
- 238000005507 spraying Methods 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 15
- 238000007664 blowing Methods 0.000 claims description 6
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 claims description 4
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- 238000013019 agitation Methods 0.000 abstract 1
- 238000005243 fluidization Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 79
- 239000007921 spray Substances 0.000 description 22
- 239000012530 fluid Substances 0.000 description 13
- 239000002245 particle Substances 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 12
- 239000000243 solution Substances 0.000 description 12
- 238000002347 injection Methods 0.000 description 10
- 239000007924 injection Substances 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 229910052742 iron Inorganic materials 0.000 description 6
- 239000003960 organic solvent Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 230000000630 rising effect Effects 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 4
- 229910000702 sendust Inorganic materials 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000011162 core material Substances 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000006247 magnetic powder Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000005011 phenolic resin Substances 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 102100022210 COX assembly mitochondrial protein 2 homolog Human genes 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 101000900446 Homo sapiens COX assembly mitochondrial protein 2 homolog Proteins 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 101001062854 Rattus norvegicus Fatty acid-binding protein 5 Proteins 0.000 description 1
- 235000011054 acetic acid Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- HGPXWXLYXNVULB-UHFFFAOYSA-M lithium stearate Chemical compound [Li+].CCCCCCCCCCCCCCCCCC([O-])=O HGPXWXLYXNVULB-UHFFFAOYSA-M 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910021652 non-ferrous alloy Inorganic materials 0.000 description 1
- LYRFLYHAGKPMFH-UHFFFAOYSA-N octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(N)=O LYRFLYHAGKPMFH-UHFFFAOYSA-N 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 235000011007 phosphoric acid Nutrition 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
Landscapes
- Powder Metallurgy (AREA)
- Chemical Treatment Of Metals (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
- Glanulating (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、被覆層の主成分と
なる物質を溶媒に溶解または分散させた溶液（以下、被
覆液という）を粉体に噴霧し、同時にまたはさらに乾燥
し、その被覆液に含まれる物質で粉体を被覆する方法に
関する。TECHNICAL FIELD The present invention relates to a method of spraying a solution (hereinafter referred to as a coating solution), in which a substance as a main component of a coating layer is dissolved or dispersed in a solvent, onto a powder, and simultaneously or further drying the coating. The present invention relates to a method of coating powder with a substance contained in a liquid.
【０００２】[0002]
【従来の技術】粉末冶金技術は、複雑な形状の部品をニ
アネット形状でしかも高寸法精度に製造することを可能
とし、切削コストを大幅に低減することを可能とする。
このため、粉末冶金製品が自動車部品，電気部品等に多
量に採用されている。原料となる粉体は、これらの部品
の用途や要求される特性に応じて適宜選択される。近
年、部品の特性を一層向上するために、粉体の表面を種
々の物質で被覆したものも検討されている。2. Description of the Related Art Powder metallurgy technology enables parts having a complicated shape to be manufactured in a near-net shape with high dimensional accuracy, and cutting costs can be greatly reduced.
For this reason, powder metallurgy products are widely used in automobile parts, electric parts and the like. The powder as a raw material is appropriately selected according to the application of these parts and the required characteristics. In recent years, in order to further improve the characteristics of parts, powders whose surfaces are coated with various substances have been studied.
【０００３】粉体の表面に被覆層を形成する方法として
は、被覆層の主成分となる物質を含有する被覆液を粉体
に噴霧し、さらに乾燥して被覆層を形成するのが一般的
である。図３は、粉体に被覆液を噴霧する方法で被覆層
を形成する際に、従来から使用されている装置の例を模
式的に示す断面図である。図３に示すように、容器１内
に粉体２を収容し、容器１の底部に配設した攪拌羽根３
を回転軸７を中心にして回転させて、粉体２を攪拌す
る。図３中の矢印ａは回転軸７の回転を示し、矢印ｂは
攪拌による粉体２の流れを示す。As a method for forming the coating layer on the surface of the powder, it is common to spray the coating liquid containing the substance which is the main component of the coating layer onto the powder and further dry it to form the coating layer. Is. FIG. 3 is a cross-sectional view schematically showing an example of an apparatus that has been conventionally used in forming a coating layer by a method of spraying a coating liquid on powder. As shown in FIG. 3, a stirring blade 3 that contains powder 2 in a container 1 and is arranged at the bottom of the container 1
Is rotated around the rotating shaft 7 to stir the powder 2. An arrow a in FIG. 3 indicates the rotation of the rotary shaft 7, and an arrow b indicates the flow of the powder 2 due to stirring.
【０００４】粉体の上方には、２種の流体を噴射する２
流体ノズル８が配設されている。噴霧ガス４と被覆液５
とを２流体ノズル８に供給することにより、被覆液５は
粉体２に噴霧される。被覆液５には被覆層の主成分とな
る物質が溶解または分散しているので、被覆液５を粉体
２に噴霧しつつ液を乾燥させることによって、粉体２の
表面に被覆層が形成される。類似の方法は、たとえば特
開2000-34502号公報において、フッ素化合物皮膜等を磁
石用合金粉末に被覆する際に採用されている。Two types of fluid are jetted above the powder.
A fluid nozzle 8 is provided. Spray gas 4 and coating liquid 5
By supplying and to the two-fluid nozzle 8, the coating liquid 5 is sprayed on the powder 2. Since the substance serving as the main component of the coating layer is dissolved or dispersed in the coating liquid 5, the coating liquid 5 is sprayed onto the powder 2 and dried to form a coating layer on the surface of the powder 2. To be done. A similar method is adopted, for example, in Japanese Patent Application Laid-Open No. 2000-34502 when coating the alloy powder for magnets with a fluorine compound film or the like.
【０００５】しかしながら図３に示す装置を用いた場
合、容器１内の粉体２の流れは、攪拌羽根３の回転によ
る攪拌（すなわち矢印ｂ）のみであるので、粉体２の上
方から噴霧された被覆液５を、粉体２の粒子全面に均一
に付着させることは困難である。そこで、上記の方法の
改良として、粉体工学便覧（第２版、粉体工学会編、日
刊工業新聞社刊）p375の図4.11.5に転動流動層として示
されているような装置による方法が検討されている。す
なわち図４に示すように容器１底部から流動ガス６を吹
き込みながら、被覆液５を粉体２に噴霧する装置によ
り、容器１内の粉体２が均一に被覆層を形成するように
するものである。図４中の矢印ｃは流動ガス６による粉
体２の舞い上がりを示す。However, when the apparatus shown in FIG. 3 is used, the flow of the powder 2 in the container 1 is only the stirring by the rotation of the stirring blades 3 (that is, the arrow b), so that the powder 2 is sprayed from above. It is difficult to uniformly apply the coating liquid 5 to the entire surface of the particles of the powder 2. Therefore, as an improvement of the above method, a device as shown as a rolling fluidized bed in Fig. 4.11.5 of p375 of Powder Engineering Handbook (2nd edition, edited by Powder Engineering Society, published by Nikkan Kogyo Shimbun) is used. Methods are being considered. That is, as shown in FIG. 4, a device for spraying the coating liquid 5 onto the powder 2 while blowing the flowing gas 6 from the bottom of the container 1 allows the powder 2 in the container 1 to uniformly form a coating layer. Is. The arrow c in FIG. 4 indicates the rising of the powder 2 by the flowing gas 6.
【０００６】つまりこの装置における粉体２の流れとし
ては、攪拌羽根３の回転による攪拌（すなわち矢印ｂ）
に加えて流動ガス６の吹き込みによる舞い上がり（すな
わち矢印ｃ）が発生する。 こうして舞い上がった粉体２
に被覆液５を噴霧することによって、粉体２の粒子全面
に均一な被覆層が形成される。しかしながら図４に示す
装置を用いた場合、装置全体の構造が複雑になり、設備
保全の負荷が増大する。That is, the flow of the powder 2 in this apparatus is the stirring by the rotation of the stirring blade 3 (that is, the arrow b).
In addition to the above, soaring (that is, arrow c) is generated due to the blowing of the flowing gas 6. Powder 2 soaring up
By spraying the coating liquid 5 on the surface of the powder 2, a uniform coating layer is formed on the entire surface of the particles of the powder 2. However, when the device shown in FIG. 4 is used, the structure of the entire device becomes complicated and the load of facility maintenance increases.
【０００７】[0007]
【特許文献１】特開2000-34502号公報[Patent Document 1] Japanese Patent Laid-Open No. 2000-34502
【非特許文献１】粉体工学便覧（第２版、粉体工学会
編、日刊工業新聞社刊）p375[Non-Patent Document 1] Powder Engineering Handbook (2nd edition, edited by Powder Engineering Society, published by Nikkan Kogyo Shimbun) p375
【０００８】[0008]
【発明が解決しようとする課題】本発明は上記のような
問題点を解消し、粉体の表面に被覆層を形成するにあた
って、簡便な手段で粉体全体に均一な被覆層を形成する
方法を提供することを目的とする。DISCLOSURE OF THE INVENTION The present invention solves the above problems and a method of forming a uniform coating layer on the entire surface of the powder by a simple means when forming the coating layer on the surface of the powder. The purpose is to provide.
【０００９】[0009]
【課題を解決するための手段】本発明者らは、粉体を収
容した容器の底部で攪拌羽根を回転させながら、粉体の
上方から流動用ガスを噴射して、攪拌羽根の回転速度と
流動用ガスの流速が粉体の攪拌および舞い上がりに及ぼ
す影響について鋭意検討した。その結果、 攪拌羽根の先
端部の回転速度および流動用ガスを粉体中に吹き込む流
速（すなわち粉体と流動ガスが接触する位置における流
速）を所定の範囲内に調整することによって、粉体全体
に均一な被覆層を形成できることを見出した。本発明
は、この知見に基づいてなされたものである。Means for Solving the Problems The inventors of the present invention injected a flowing gas from above the powder while rotating the stirring blade at the bottom of the container containing the powder, thereby controlling the rotation speed of the stirring blade. The influence of the flow velocity of the flowing gas on the stirring and rising of the powder was investigated. As a result, by adjusting the rotation speed of the tip of the stirring blade and the flow velocity for blowing the flowing gas into the powder (that is, the flow velocity at the position where the powder and the flowing gas come into contact) within a predetermined range, It was found that a uniform coating layer can be formed on the surface. The present invention has been made based on this finding.
【００１０】本発明は、容器内に粉体を収容し、容器の
底部に配設した攪拌羽根を先端部の回転速度 1.5ｍ／se
c 以上で回転させるとともに、粉体の上方から流動用ガ
スを噴射して 3.0ｍ／sec 以上の流速で流動用ガスを粉
体中に吹き込むことによって粉体を攪拌流動させて、粉
体の上方から被覆液を噴霧，乾燥させることによって被
覆層を形成する粉体の被覆方法である。According to the present invention, the powder is housed in a container, and the stirring blade disposed at the bottom of the container is rotated at a tip speed of 1.5 m / se.
While rotating above c, the flow gas is sprayed from above the powder, and the flow gas is blown into the powder at a flow rate of 3.0 m / sec or more to stir and flow the powder. It is a method of coating a powder by forming a coating layer by spraying and drying the coating liquid from the above.
【００１１】前記した発明においては、好適態様とし
て、攪拌羽根を先端部の回転速度 1.5〜30ｍ／sec で回
転させ、かつ流動用ガスを 3.0〜500 ｍ／sec の流速で
粉体に吹き込むことが好ましい。また、粉体が、鉄粉ま
たは鋼粉であって、被覆液が第１リン酸アルミニウム水
溶液であることが好ましい。In a preferred embodiment of the above-mentioned invention, the stirring blade is rotated at a tip speed of 1.5 to 30 m / sec, and a flowing gas is blown into the powder at a flow rate of 3.0 to 500 m / sec. preferable. Further, it is preferable that the powder is iron powder or steel powder, and the coating liquid is an aqueous solution of primary aluminum phosphate.
【００１２】[0012]
【発明の実施の形態】本発明の方法で被覆される粉体は
特に限定しないが、平均粒径が約10〜150 μｍ程度、嵩
密度が 1.0〜4.5 ｇ／cm3 程度のものが特に好適であ
る。具体的な例としては、アトマイズ鉄粉，還元鉄粉，
鉄基合金鋼粉，ステンレス粉，およびアルミニウム粉や
銅粉等の非鉄金属粉，非鉄合金鋼粉，ならびにセラミッ
クやガラス等の無機化合物粉末等が挙げられる。BEST MODE FOR CARRYING OUT THE INVENTION The powder coated by the method of the present invention is not particularly limited, but those having an average particle size of about 10 to 150 μm and a bulk density of about 1.0 to 4.5 g / cm 3 are particularly preferable. Is. Specific examples include atomized iron powder, reduced iron powder,
Examples include iron-based alloy steel powder, stainless powder, non-ferrous metal powder such as aluminum powder and copper powder, non-ferrous alloy steel powder, and inorganic compound powder such as ceramics and glass.
【００１３】また、被覆層の組成についても、被覆液に
て塗布可能なものであれば特に限定はない。ここで、被
覆層を形成する物質は水や有機溶媒等の液に溶解あるい
は分散（エマルジョン，サスペンション等の懸濁状も含
む）させ、被覆液とする。そして水，有機溶媒等を乾燥
工程にて蒸発させる。有機溶媒の場合、揮発性が高いも
のが好ましい。The composition of the coating layer is not particularly limited as long as it can be applied with the coating liquid. Here, the substance forming the coating layer is dissolved or dispersed in a liquid such as water or an organic solvent (including suspension such as emulsion and suspension) to obtain a coating liquid. Then, water, organic solvent and the like are evaporated in the drying process. In the case of the organic solvent, those having high volatility are preferable.
【００１４】粉体への被覆の例としては、粉体として鉄
粉やセンダスト粉末等の軟磁性粉末を使用し、被覆液と
してエポキシ樹脂やフェノール樹脂等をＭＥＫ（メチル
エチルケトン）やトルエン等の有機溶媒に溶かした溶液
を用いて、粉体粒子表面に絶縁性の高い樹脂層を形成す
ることができる。このような粉末は、低損失の磁心材料
用の原料とすることができる。As an example of coating the powder, a soft magnetic powder such as iron powder or sendust powder is used as the powder, and an epoxy resin, a phenol resin or the like is used as the coating liquid in an organic solvent such as MEK (methyl ethyl ketone) or toluene. A resin layer having a high insulating property can be formed on the surface of the powder particles by using the solution dissolved in. Such powder can be used as a raw material for a low-loss magnetic core material.
【００１５】また、同じく磁心材料用原料向けの用途で
は、被覆液として、クロム酸，リン酸，シュウ酸，酢
酸，ギ酸、あるいはMg，Ｂ，Ca，Al等の金属元素を含む
これらの酸の塩を水やエタノール等の有機溶媒に溶かし
た溶液を用いて、鉄粉等の軟磁性粉末の表面に絶縁層を
形成することも、本発明の方法によれば可能である。さ
らに、粉体として鉄粉やステンレス粉末等の焼結部品原
料粉を用い、被覆液として金属石鹸（たとえばステアリ
ン酸亜鉛やステアリン酸リチウム）や脂肪酸アミド（た
とえばステアリン酸アミド）等の潤滑剤をエマルジョン
化して水等の液状媒体に分散させたものを用いることに
よって、粉体粒子表面に潤滑剤が均一に被覆され、金型
成形時の摩擦抑制の効果が顕著に改善される。Similarly, in applications for raw materials for magnetic core materials, chromic acid, phosphoric acid, oxalic acid, acetic acid, formic acid, or these acids containing metal elements such as Mg, B, Ca and Al are used as coating liquids. It is also possible according to the method of the present invention to form an insulating layer on the surface of a soft magnetic powder such as iron powder using a solution in which a salt is dissolved in an organic solvent such as water or ethanol. In addition, powdered raw material of sintered parts such as iron powder or stainless powder is used as powder, and a lubricant such as metal soap (eg, zinc stearate or lithium stearate) or fatty acid amide (eg, stearic acid amide) is emulsified as coating liquid. By using a material which is made into a liquid and dispersed in a liquid medium such as water, the surface of the powder particles is uniformly coated with the lubricant, and the effect of suppressing friction during die molding is remarkably improved.
【００１６】無論、 本発明は上記の用途に限定されるも
のではない。なお、被覆液中の被覆層を形成する物質の
濃度は 0.5〜20質量％程度が好適である。以下に、本発
明の方法を詳しく説明する。図１は、本発明を適用する
装置の例を模式的に示す断面図である。図１に示すよう
に、容器１内に粉体２を収容し、容器１の底部近傍に配
設した攪拌羽根３を回転軸７を中心にして回転させて、
粉体２を攪拌する。図１中の矢印ａは回転軸７の回転を
示し、矢印ｂは攪拌による粉体２の流れを示す。Of course, the invention is not limited to the above applications. The concentration of the substance forming the coating layer in the coating liquid is preferably about 0.5 to 20% by mass. Hereinafter, the method of the present invention will be described in detail. FIG. 1 is a sectional view schematically showing an example of an apparatus to which the present invention is applied. As shown in FIG. 1, the powder 2 is contained in a container 1, and a stirring blade 3 arranged near the bottom of the container 1 is rotated about a rotation shaft 7 to
Stir the powder 2. The arrow a in FIG. 1 indicates the rotation of the rotary shaft 7, and the arrow b indicates the flow of the powder 2 due to stirring.
【００１７】ここで攪拌羽根３の直径は 100〜2000mm程
度、容器１の内径（底面の断面形状が非円形の場合は内
接する円の径）は攪拌羽根３の約 1.0〜1.5 倍とするこ
とが好ましい。なお、容器１は略円筒状が好ましい。容
器１への粉体２の充填量は、粉体層の厚み（充填される
高さ）が攪拌羽根３の直径の１／２以下とすることが好
ましい。Here, the diameter of the stirring blade 3 is about 100 to 2000 mm, and the inner diameter of the container 1 (the diameter of the circle inscribed when the bottom surface has a non-circular cross section) is about 1.0 to 1.5 times that of the stirring blade 3. Is preferred. The container 1 preferably has a substantially cylindrical shape. The amount of the powder 2 filled in the container 1 is preferably such that the thickness of the powder layer (filling height) is 1/2 or less of the diameter of the stirring blade 3.
【００１８】さて、本発明者らは、攪拌羽根３の回転が
粉体２の攪拌に及ぼす影響を調査した。すなわち粉体２
としてアトマイズ純鉄粉（川崎製鉄（株）製 KIP-304A
S）を容器１内に収容し、後述する噴霧ガス４や流動ガ
ス６を使用せず、粉体２を静止させた後、 攪拌羽根３を
30秒間回転させた。容器１内に収容した粉体２は２kg，
20kg，200kg とし、それぞれ１質量％の染料を加えて攪
拌羽根３の回転数を種々変化させて、粉体２の混合状態
を目視で観察した。ここで、容器１としては、回転羽根
径の約 1.1倍の直径を有する略円形のものを、それぞれ
用いた。The present inventors investigated the influence of the rotation of the stirring blade 3 on the stirring of the powder 2. That is, powder 2
As atomized pure iron powder (KIP-304A manufactured by Kawasaki Steel Co., Ltd.)
S) is housed in the container 1, the spraying gas 4 and the flowing gas 6 described later are not used, and the powder 2 is allowed to stand still.
It was rotated for 30 seconds. The powder 2 contained in the container 1 is 2 kg,
The amounts of the powder 2 were 20 kg and 200 kg, respectively, and 1% by mass of the dye was added thereto, and the rotation speed of the stirring blade 3 was variously changed to visually observe the mixed state of the powder 2. Here, as the container 1, a substantially circular container having a diameter of about 1.1 times the diameter of the rotating blade was used.
【００１９】その結果を表１に示す。The results are shown in Table 1.
【００２０】[0020]
【表１】 [Table 1]
【００２１】表１から明らかなように、攪拌羽根３の先
端部の回転速度が 1.5ｍ／sec 以上であれば粉体２は容
器１内で十分に攪拌され、均一に混合されることが確認
できた。つまり攪拌羽根３の先端部の回転速度を 1.5ｍ
／sec 以上とする必要がある。 ただし粉体２の粒子の強
度および靭性によっては、回転速度が30ｍ／sec を超え
ると、せん断力により粒子が変形あるいは分解して、粉
体２の粉体特性が大きく変化するので好ましくない。し
たがって、攪拌羽根３の先端部の回転速度は 1.5〜30ｍ
／sec が好ましい。As is clear from Table 1, it was confirmed that the powder 2 was sufficiently stirred in the container 1 and uniformly mixed if the rotation speed of the tip of the stirring blade 3 was 1.5 m / sec or more. did it. That is, the rotation speed of the tip of the stirring blade 3 is 1.5 m
/ Sec or more is required. However, depending on the strength and toughness of the particles of the powder 2, if the rotation speed exceeds 30 m / sec, the particles are deformed or decomposed by the shearing force, and the powder characteristics of the powder 2 are greatly changed, which is not preferable. Therefore, the rotation speed of the tip of the stirring blade 3 is 1.5 to 30 m.
/ Sec is preferred.
【００２２】図１に示すように、本発明の方法において
は、さらに粉体２の上方には、２流体ノズル８と流動ガ
ス噴射ノズル９が配設される。この２流体ノズル８は、
噴霧ガス４とともに被覆液５を粉体２に噴霧する。被覆
液５には被覆層の主成分となる物質が溶解または分散し
ているので、被覆液５を粉体２に噴霧，乾燥させること
によって、粉体２の表面に被覆層が形成される。なお、
被覆液５の噴霧量は粉体１kgあたり１〜100 mg／sec 程
度が好ましい。As shown in FIG. 1, in the method of the present invention, a two-fluid nozzle 8 and a flowing gas injection nozzle 9 are arranged above the powder 2. This two-fluid nozzle 8
The coating liquid 5 is sprayed onto the powder 2 together with the spray gas 4. Since the substance serving as the main component of the coating layer is dissolved or dispersed in the coating liquid 5, the coating layer 5 is formed on the surface of the powder 2 by spraying and drying the coating liquid 5 on the powder 2. In addition,
The spray amount of the coating liquid 5 is preferably about 1 to 100 mg / sec per 1 kg of powder.
【００２３】一方、流動ガス噴射ノズル９は流動ガス６
を粉体２に噴射して、粉体２の舞い上がり（すなわち矢
印ｃ）を発生させる。この場合、流動ガス６は流動用ガ
スとして働く。流動ガス６および噴霧ガス４としては、
一般の空気で良いが、 用途によっては窒素ガス等の不活
性ガスを用いても良い。また、これらのガスは、通常、
室温とするが、用途により流動ガス６の温度を制御して
も良い。On the other hand, the fluidized gas injection nozzle 9 has a fluidized gas 6
Is sprayed onto the powder 2 to cause the powder 2 to rise (that is, the arrow c). In this case, the flowing gas 6 acts as a flowing gas. As the flowing gas 6 and the atomizing gas 4,
Ordinary air may be used, but depending on the application, an inert gas such as nitrogen gas may be used. Also, these gases are usually
Although the temperature is set to room temperature, the temperature of the flowing gas 6 may be controlled depending on the application.
【００２４】さて、本発明者らは、流動ガス６の噴射が
粉体２の流動に及ぼす影響を調査した。すなわち粉体２
として上記の実験と同じアトマイズ純鉄粉を容器１内
（水平断面が直径約180mm の略円形）に収容し、攪拌羽
根３を使用せず、粉体２を静止させた後、 流動ガス噴射
ノズル９を粉体２の上面に接する位置に固定して、室温
の空気を流動ガス６として噴射した。つまり、このとき
の流動ガス６の流速は、流動ガス６が粉体２に接触する
位置における流速（すなわち流動ガス６を粉体２中に吹
き込む流速）である。このようにして、流動ガス噴射ノ
ズル９の噴射口の面積を1.04mm2 ，13.9mm2 ，55.0mm2
とし、流動ガス６の流量を種々変化させて、粉体２の舞
い上がりの有無を目視で観察した。その結果を表２に示
す。Now, the present inventors investigated the influence of the injection of the flowing gas 6 on the flow of the powder 2. That is, powder 2
As above, the same atomized pure iron powder as in the above experiment was placed in the container 1 (horizontal cross-section is approximately circular with a diameter of about 180 mm), the stirring blade 3 was not used, and the powder 2 was left stationary. 9 was fixed at a position in contact with the upper surface of the powder 2, and air at room temperature was sprayed as the flowing gas 6. That is, the flow velocity of the fluidizing gas 6 at this time is the flow velocity at the position where the fluidizing gas 6 contacts the powder 2 (that is, the velocity at which the fluidizing gas 6 is blown into the powder 2). In this way, 1.04 mm 2 area of the injection port of the fluidizing gas injection nozzles 9, 13.9mm 2, 55.0mm 2
Then, the flow rate of the flowing gas 6 was variously changed and the presence or absence of the rising of the powder 2 was visually observed. The results are shown in Table 2.
【００２５】[0025]
【表２】 [Table 2]
【００２６】表２から明らかなように、流動ガス６を粉
体２中に吹き込む流速が 3.0ｍ／sec 以上であれば粉体
２の舞い上がりが認められた。つまり流動ガス６の流速
を 3.0ｍ／sec 以上とする必要がある。 ただし流速が 5
00ｍ／min を超えると、流動ガス６の噴射装置の負荷が
増大して設備故障の原因になる。したがって、流動ガス
６を粉体２中に吹き込む流速は 3.0〜500 ｍ／sec が好
ましい。As is clear from Table 2, when the flow velocity of the flowing gas 6 into the powder 2 was 3.0 m / sec or more, the powder 2 was seen to rise. That is, it is necessary to set the flow velocity of the flowing gas 6 to 3.0 m / sec or more. However, the flow velocity is 5
If it exceeds 00 m / min, the load of the fluid gas injection device increases, causing equipment failure. Therefore, the flow velocity of the flowing gas 6 blown into the powder 2 is preferably 3.0 to 500 m / sec.
【００２７】本発明においては、攪拌羽根３と流動ガス
６とによって粉体２の攪拌と舞い上がりとを同時に発生
（以下、攪拌流動という）させて、２流体ノズル８から
被覆液５を噴霧する。これにより粉体２の粒子全面に被
覆液５を被覆でき、均一な被覆層を形成できる。なお、
図１に示すように、２流体ノズル８と流動ガス噴射ノズ
ル９を設け、 ２流体ノズル８の噴霧ガス４の流量と流動
ガス６の流量を両方増加して、粉体２の舞い上がり（す
なわち矢印ｃ）を発生させても良い。この場合は、噴霧
ガス４と流動ガス６の両方が流動用ガスとして働く。In the present invention, the stirring blade 3 and the flowing gas 6 simultaneously generate and stir the powder 2 (hereinafter referred to as stirring flow), and the coating liquid 5 is sprayed from the two-fluid nozzle 8. As a result, the entire surface of the particles of the powder 2 can be coated with the coating liquid 5, and a uniform coating layer can be formed. In addition,
As shown in FIG. 1, a two-fluid nozzle 8 and a flowing gas injection nozzle 9 are provided, and both the flow rate of the spray gas 4 and the flow rate of the flowing gas 6 of the two-fluid nozzle 8 are increased so that the powder 2 rises (that is, the arrow c) may be generated. In this case, both the spray gas 4 and the flowing gas 6 work as a flowing gas.
【００２８】また図２に示すように、流動ガス噴射ノズ
ル９を設けず、２流体ノズル８のみを用い、２流体ノズ
ル８の噴霧ガス４の流量を増加して、粉体２の舞い上が
り（すなわち矢印ｃ）を発生させても良い。この場合
は、噴霧ガス４が流動用ガスとして働く。図２中の他の
記号は、図１と同じである。ここで、流動ガス６（およ
び噴霧ガス４）を粉体に吹き込む位置は、任意に設定す
ることができるが、図１および図２に示すように攪拌羽
根３の先端部近傍（すなわち攪拌羽根３による攪拌が最
も活発な領域）に上方より吹き込むと、舞い上がりが効
率良く発生するため好ましい。また被覆液５は、舞い上
がりが発生している領域に向けて噴霧することが好まし
い。Further, as shown in FIG. 2, the fluidized gas injection nozzle 9 is not provided and only the two-fluid nozzle 8 is used to increase the flow rate of the spray gas 4 of the two-fluid nozzle 8 to raise the powder 2 (that is, The arrow c) may be generated. In this case, the atomizing gas 4 works as a flowing gas. Other symbols in FIG. 2 are the same as those in FIG. Here, the position where the flowing gas 6 (and the spray gas 4) is blown into the powder can be set arbitrarily, but as shown in FIGS. 1 and 2, the vicinity of the tip of the stirring blade 3 (that is, the stirring blade 3). It is preferable to blow the mixture into the region (where the stirring is most active) from above because the rising is efficiently generated. Further, it is preferable that the coating liquid 5 is sprayed toward the region where the rising is occurring.
【００２９】本発明では、容器１底部には流動ガス６の
配管や吹き込み装置を配設する必要はない。また噴霧を
行なう部分の粉体２を舞い上がらせれば良いため、流動
ガス６の流量は少なくて良い。したがって簡便な手段
で、被覆液５を粉体２全体に均一に付着，乾燥させるこ
とによって、粉体２表面に被覆層が形成される。以下、
乾燥工程について説明する。被覆液５が噴霧された個々
の粉体２粒子は、他の粒子が噴霧されている間も流動す
るガスに触れるので、噴霧工程中に乾燥も進行する。し
かし、乾燥を促進するために、噴霧ガス４および／また
は流動ガス６を加熱して送風する方法や、容器１を加熱
する方法等が使用でき、またこれらの方法を併用しても
良い。In the present invention, it is not necessary to provide a pipe or a blowing device for the flowing gas 6 at the bottom of the container 1. Further, since the powder 2 in the portion to be sprayed may be raised, the flow rate of the flowing gas 6 may be small. Therefore, a coating layer 5 is formed on the surface of the powder 2 by uniformly attaching and drying the coating liquid 5 on the entire powder 2 by a simple means. Less than,
The drying process will be described. The individual particles of the powder 2 sprayed with the coating liquid 5 come into contact with the flowing gas even while the other particles are sprayed, so that the drying also progresses during the spraying process. However, in order to accelerate the drying, a method of heating the spray gas 4 and / or the flowing gas 6 to blow air, a method of heating the container 1 or the like can be used, and these methods may be used in combination.
【００３０】乾燥を促進する方法としては、容器１を加
熱することにより、粉体２を加熱する方法が好ましい。
ただし、粉体２の融点が加熱温度より高い場合に限る。
粉体２自体を加熱することにより、乾燥に必要なガスの
流量を少なくすることができ、装置の構造を簡略化でき
る。容器１自体の加熱方法としては、容器１自体に蒸気
やオイル等の熱媒体を循環させる方法や、容器１にリボ
ンヒーターを巻き付けて加熱する方法等がある。粉体２
の加熱温度としては50〜200 ℃が好ましい。As a method for promoting the drying, it is preferable to heat the powder 2 by heating the container 1.
However, only when the melting point of the powder 2 is higher than the heating temperature.
By heating the powder 2 itself, the flow rate of gas required for drying can be reduced, and the structure of the device can be simplified. As a method of heating the container 1 itself, there are a method of circulating a heat medium such as steam and oil in the container 1 itself, and a method of winding a ribbon heater around the container 1 to heat the container 1. Powder 2
The heating temperature is preferably 50 to 200 ° C.
【００３１】このような方法を使用することによって、
被覆液５の溶媒の乾燥による被覆層の形成を噴霧工程と
同時期に行なうことが可能である。他方、噴霧の終了後
も攪拌を継続することにより、追加の乾燥工程を加え、
乾燥を確実なものとしても良い。後者の場合、流動ガス
６による攪拌は、乾燥期も継続することが好ましい。ま
た、噴霧を終了後も攪拌を継続する場合は、必要に応じ
て攪拌羽根３の回転数を増減しても良い。噴霧ガスおよ
び／または流動ガス６の加熱や、容器１の加熱も無論採
用可能である。By using such a method,
It is possible to form the coating layer by drying the solvent of the coating liquid 5 at the same time as the spraying step. On the other hand, by continuing the stirring after the end of spraying, an additional drying step is added,
Drying may be assured. In the latter case, it is preferable that the stirring with the fluidized gas 6 is continued during the drying period. If the stirring is continued after the spraying is finished, the rotation speed of the stirring blade 3 may be increased or decreased as necessary. Of course, the heating of the atomizing gas and / or the flowing gas 6 and the heating of the container 1 can be adopted.
【００３２】[0032]
【実施例】以下、 実施例によってさらに詳細に本発明に
ついて説明するが、本発明の主旨は以下の例の具体的条
件に拘束されるものではない。
（実施例１）表３の発明例１〜５，10，11および比較例
１〜５では、図２に示す装置を用い、粉体２としてアト
マイズ純鉄粉（川崎製鉄（株）製 KIP-304AS；平均粒径
75μｍ，見掛け密度 3.0Mg／ｍ3 ）およびセンダスト粉
末（主成分Fe，Al，Si、平均粒径53μｍ，見掛け密度2.
24Mg／ｍ3 ）を使用した。また、被覆液５としてアセト
ンを溶媒とした濃度20質量％のフェノール樹脂溶液およ
びアセトンを溶媒とした濃度20質量％のエポキシ樹脂溶
液を使用した。The present invention will be described in more detail with reference to the following examples, but the gist of the present invention is not limited to the specific conditions of the following examples. (Example 1) In Invention Examples 1 to 5, 10 and 11 of Table 3 and Comparative Examples 1 to 5, the apparatus shown in FIG. 2 was used, and atomized pure iron powder (KIP-made by Kawasaki Steel Co., Ltd.) was used as the powder 2. 304AS ； Average particle size
75μm, apparent density 3.0Mg / m 3 ) and sendust powder (main component Fe, Al, Si, average particle size 53μm, apparent density 2.
24 Mg / m 3 ) was used. Further, as the coating liquid 5, a phenol resin solution having a concentration of 20 mass% using acetone as a solvent and an epoxy resin solution having a concentration of 20 mass% using acetone as a solvent were used.
【００３３】上記の粉体２を容器１に充填し、攪拌羽根
３の先端部の回転速度と噴霧ガス４を粉体２中に吹き込
む流速とを種々変化させて、20kgの粉体２を攪拌流動さ
せながら、被覆液５を粉体２の上方から 900秒間噴霧し
た。次いで、被覆液５の噴霧を停止して攪拌羽根３の回
転と噴霧ガス４の噴射を 300秒間継続して乾燥し、被覆
層を形成した。The powder 2 described above is filled in the container 1, and the rotational speed of the tip of the stirring blade 3 and the flow velocity of the spray gas 4 blown into the powder 2 are variously changed to agitate 20 kg of the powder 2. The coating liquid 5 was sprayed from above the powder 2 for 900 seconds while flowing. Next, the spraying of the coating liquid 5 was stopped, the rotation of the stirring blade 3 and the spraying of the spray gas 4 were continued for 300 seconds to dry, and a coating layer was formed.
【００３４】上記の被覆工程の終了後、装置から粉体２
を取り出し、 200℃で60分間加熱して樹脂の硬化処理を
行なった。なお、容器１は、直径が300mm の略円形の水
平断面のもの（すなわち略円筒状のもの）を使用し、攪
拌羽根３の羽根直径は280mm とした。また、流動ガス６
を兼ねる噴霧ガス４は、室温の空気を使用した。被覆液
５の時間あたりの噴霧量は400mg／sec とした。After the above coating process is completed, the powder 2 is discharged from the apparatus.
Was taken out and heated at 200 ° C. for 60 minutes to cure the resin. As the container 1, a substantially circular horizontal section having a diameter of 300 mm (that is, a substantially cylindrical shape) was used, and the blade diameter of the stirring blade 3 was 280 mm. In addition, flowing gas 6
Air at room temperature was used as the atomizing gas 4 that also serves as the above. The amount of the coating liquid 5 sprayed per hour was 400 mg / sec.
【００３５】表３の発明例６〜９では、図１に示す装置
を用い、粉体２として発明例１と同様の鉄粉（川崎製鉄
（株）製 KIP-304AS）およびセンダスト粉末を使用し
た。また、被覆液５としてアセトンを溶媒とした濃度20
質量％のフェノール樹脂溶液を使用した。上記の粉体２
を容器１に充填し、攪拌羽根３の先端部の回転速度を一
定（＝5.00ｍ／sec ）で、噴霧ガス４と流動ガス６を20
kgの粉体２中に吹き込む速度を種々変化させて、粉体２
を攪拌流動させながら、被覆液５を粉体２の上方から 9
00秒間噴霧した。次いで、被覆液５と噴霧ガス４の噴霧
を停止して、攪拌羽根３の回転と流動ガス６の噴射を 3
00秒間継続して乾燥し、被覆層を形成した。ノズルは発
明例１と同様のものを用いた。また流動ガス６と噴霧ガ
ス４は、ともに室温の空気を用いた。In Invention Examples 6 to 9 in Table 3, the same apparatus as in Invention Example 1 (KIP-304AS manufactured by Kawasaki Steel Co., Ltd.) and Sendust powder were used as the powder 2 using the apparatus shown in FIG. . Also, the concentration of the coating liquid 5 using acetone as a solvent is 20
A mass% phenolic resin solution was used. Powder 2 above
Is charged in a container 1, and the atomizing gas 4 and the flowing gas 6 are kept at a constant rotational speed (= 5.00 m / sec) at the tip of the stirring blade 3.
By changing the blowing speed into the powder 2 of kg,
While stirring and flowing, the coating liquid 5 is applied from above the powder 2 9
Sprayed for 00 seconds. Then, the spraying of the coating liquid 5 and the spray gas 4 is stopped, and the rotation of the stirring blade 3 and the injection of the flowing gas 6 are stopped.
It was continuously dried for 00 seconds to form a coating layer. The nozzle used was the same as that used in Inventive Example 1. Air at room temperature was used for both the flowing gas 6 and the spray gas 4.
【００３６】上記の被覆工程の終了後、装置から粉体２
を取り出し、 200℃で60分間加熱して被覆層中の樹脂の
硬化処理を行なった。このようにして得られた被覆層を
有する粉体２を980MPaで加圧成形し、リング形状（外径
38mm，内径25mm，厚さ6.2mm ）の試料を作製した。次
に、これらの試料の比抵抗（μΩｍ）を、四端子法で測
定した。その結果を表３に示す。なお、比抵抗が大きい
ほど、粉体２の絶縁性が優れており、均一な被覆層が形
成されたことを示している。After the above coating process is completed, the powder 2 is discharged from the apparatus.
Was taken out and heated at 200 ° C. for 60 minutes to cure the resin in the coating layer. The powder 2 having the coating layer thus obtained was pressure-molded at 980 MPa to give a ring shape (outer diameter:
A sample with a diameter of 38 mm, an inner diameter of 25 mm, and a thickness of 6.2 mm was prepared. Next, the specific resistance (μΩm) of these samples was measured by the four-terminal method. The results are shown in Table 3. It should be noted that the larger the specific resistance is, the more excellent the insulating property of the powder 2 is, which means that the uniform coating layer is formed.
【００３７】[0037]
【表３】 [Table 3]
【００３８】発明例１〜11は、攪拌羽根３先端部の回転
速度と流動用ガス（すなわち噴霧ガス４および／または
流動ガス６）の流速が本発明の範囲を満足する例であ
る。比較例１は、攪拌羽根３を停止しかつ噴霧ガス４の
流速が本発明の範囲を外れる例であり、比較例２は、攪
拌羽根３先端部の回転速度と噴霧ガス４の流速が本発明
の範囲を外れる例であり、比較例３は、攪拌羽根３先端
部の回転速度が本発明の範囲を外れる例であり、比較例
４は、噴霧ガス４の流速が本発明の範囲を外れる例であ
る。Inventive Examples 1 to 11 are examples in which the rotational speed of the tip of the stirring blade 3 and the flow velocity of the flowing gas (that is, the spray gas 4 and / or the flowing gas 6) satisfy the range of the present invention. Comparative Example 1 is an example in which the stirring blade 3 is stopped and the flow velocity of the spray gas 4 is outside the range of the present invention. In Comparative Example 2, the rotation speed of the tip of the stirring blade 3 and the flow velocity of the spray gas 4 are the present invention. Comparative Example 3 is an example in which the rotation speed of the tip of the stirring blade 3 is out of the range of the present invention, and Comparative Example 4 is an example in which the flow velocity of the spray gas 4 is out of the range of the present invention. Is.
【００３９】鉄粉を粉体２とした発明例１〜９および11
では比抵抗が3060〜4270μΩｍであったのに対して、同
じ鉄粉を粉体２とした比較例１〜４では20〜2450μΩｍ
であった。また、センダスト粉末を粉体２とした発明例
10と比較例５でも、発明例10の方が２倍程度高い比抵抗
を示した。したがって、本発明の被覆方法で被覆層を形
成した粉体は比抵抗が大きいので、均一な被覆層が形成
されていることが確かめられた。Invention Examples 1 to 9 and 11 in which iron powder is powder 2
In contrast, the specific resistance was 3060 to 4270 μΩm, whereas in Comparative Examples 1 to 4 in which the same iron powder was powder 2, 20 to 2450 μΩm.
Met. Inventive example in which Sendust powder is powder 2
Also in 10 and Comparative Example 5, Inventive Example 10 exhibited about twice higher specific resistance. Therefore, it was confirmed that the powder having the coating layer formed by the coating method of the present invention had a large specific resistance, and thus a uniform coating layer was formed.
【００４０】（実施例２）表４の発明例12〜15および比
較例６〜８では、粉末２として発明例１と同じアトマイ
ズ純鉄粉，被覆液５として濃度10質量％のリン酸エタノ
ール溶液および濃度10質量％の第１リン酸アルミニウム
水溶液を使用し、噴霧液５の噴霧量を 300mg／sec ，噴
霧時間を2000秒とし、その他の条件は発明例１と同様と
して、粒子表面に絶縁被覆層が形成された鉄粉２を製造
した。なお、リン酸エタノール溶液を噴霧した場合は、
溶液中のリン酸が鉄粉２表面で化学反応を起こして絶縁
被覆層を形成する。(Example 2) In Invention Examples 12 to 15 and Comparative Examples 6 to 8 in Table 4, the powder 2 is the same atomized pure iron powder as in Invention Example 1, and the coating solution 5 is an ethanol solution of phosphoric acid having a concentration of 10% by mass. And 10% by mass aqueous solution of monobasic aluminum phosphate were used, the spray amount of spray liquid 5 was 300 mg / sec, the spray time was 2000 seconds, and the other conditions were the same as in Inventive Example 1, and the particle surface was coated with an insulating coating. A layered iron powder 2 was produced. In addition, when spraying the ethanolic phosphate solution,
Phosphoric acid in the solution causes a chemical reaction on the surface of the iron powder 2 to form an insulating coating layer.
【００４１】その後、 製造された被覆層を有する鉄粉２
を、実施例１と同様の方法で、外径38mm，内径25mm，厚
さ6.2mm のリング形状に成形した。これらリング形状試
料の比抵抗（μΩｍ）を、四端子法で測定した結果を表
４に示す。なお、比抵抗が大きい程、粉体２の絶縁性が
優れており、均一な被覆が形成されたことを示してい
る。After that, the iron powder 2 having the produced coating layer
Was molded into a ring shape having an outer diameter of 38 mm, an inner diameter of 25 mm and a thickness of 6.2 mm by the same method as in Example 1. Table 4 shows the results of measuring the specific resistance (μΩm) of these ring-shaped samples by the four-terminal method. It should be noted that the larger the specific resistance is, the more excellent the insulating property of the powder 2 is, which means that the uniform coating is formed.
【００４２】[0042]
【表４】 [Table 4]
【００４３】発明例12〜15は、攪拌羽根３先端部の回転
速度と流動用ガス（すなわち噴霧ガス４および／または
流動ガス６）の流速が、本発明の範囲を満足している例
である。比較例６は、攪拌羽根３先端部の回転速度が本
発明の範囲を外れる例であり、比較例７および８は、噴
霧ガス４の流速が本発明の範囲を外れる例である。リン
酸を被覆液５とした発明例12および13では比抵抗が50〜
60μΩｍであったのに対して、比較例６および８では12
〜14μΩｍであった。また、第１リン酸アルミニウムを
被覆液５とした発明例14および15では比抵抗が 467〜47
3 μΩｍであったのに対して、比較例７では 225μΩｍ
であった。したがって、本発明の方法で被覆層を形成し
た粉体２は、比抵抗が大きいので、均一な被覆層が形成
されていることが分かる。Invention Examples 12 to 15 are examples in which the rotational speed of the tip of the stirring blade 3 and the flow velocity of the flowing gas (ie, the spray gas 4 and / or the flowing gas 6) satisfy the range of the present invention. . Comparative Example 6 is an example in which the rotational speed of the tip of the stirring blade 3 is out of the range of the present invention, and Comparative Examples 7 and 8 are examples in which the flow velocity of the spray gas 4 is out of the range of the present invention. In Invention Examples 12 and 13 using phosphoric acid as the coating liquid 5, the specific resistance was 50 to
While it was 60 μΩm, it was 12 in Comparative Examples 6 and 8.
It was ˜14 μΩm. Further, in Invention Examples 14 and 15 in which the coating solution 5 was monoaluminum phosphate, the specific resistance was 467 to 47.
It was 3 μΩm, whereas in Comparative Example 7, it was 225 μΩm
Met. Therefore, it can be seen that the powder 2 having the coating layer formed by the method of the present invention has a large specific resistance, and thus a uniform coating layer is formed.
【００４４】本発明の方法で均一な絶縁被覆層を施した
これらの鉄粉等の軟磁性粉末は、損失（鉄損）の小さい
磁心を製造するための原料として好適である。These soft magnetic powders such as iron powders, which are provided with a uniform insulating coating layer by the method of the present invention, are suitable as a raw material for producing a magnetic core having a small loss (iron loss).
【００４５】[0045]
【発明の効果】本発明によれば、 簡便な装置で粉体全体
に均一な被覆層を形成できる。According to the present invention, a uniform coating layer can be formed on the entire powder by a simple device.
【図１】本発明を適用する装置の例を模式的に示す断面
図である。FIG. 1 is a sectional view schematically showing an example of an apparatus to which the present invention is applied.
【図２】本発明を適用する装置の他の例を模式的に示す
断面図である。FIG. 2 is a sectional view schematically showing another example of an apparatus to which the present invention is applied.
【図３】従来の装置の例を模式的に示す断面図である。FIG. 3 is a cross-sectional view schematically showing an example of a conventional device.
【図４】従来の装置の他の例を模式的に示す断面図であ
る。FIG. 4 is a sectional view schematically showing another example of a conventional device.
１ 容器 ２ 粉体 ３ 攪拌羽根 ４ 噴霧ガス ５ 被覆液 ６ 流動ガス ７ 回転軸 ８ ２流体ノズル ９ 流動ガス噴射ノズル 1 container 2 powder 3 stirring blades 4 atomizing gas 5 coating liquid 6 flowing gas 7 rotation axis 8 two-fluid nozzle 9 Fluid gas injection nozzle
───────────────────────────────────────────────────── フロントページの続き (72)発明者 植田 正輝 千葉県千葉市中央区川崎町１番地 川崎製 鉄株式会社技術研究所内 (72)発明者 斉藤 慎悟 千葉県千葉市中央区川崎町１番地 川崎製 鉄株式会社技術研究所内 Ｆターム(参考） 4D075 AA04 AA69 AA85 BB14Y BB24Z CA09 CA23 DA11 DB02 DB04 DB06 DB07 DB13 DB14 DC13 DC19 EA06 EA07 EA13 EB01 EB32 EB33 EC01 EC07 4G004 BA00 4K026 AA02 AA04 AA06 AA09 AA23 BA03 BB05 CA16 CA23 CA37 DA04 DA06 ─────────────────────────────────────────────────── ─── Continued front page (72) Inventor Masateru Ueda 1 Kawasaki-cho, Chuo-ku, Chiba-shi, Chiba Made in Kawasaki Technical Research Institute of Iron Co., Ltd. (72) Inventor Shingo Saito 1 Kawasaki-cho, Chuo-ku, Chiba-shi, Chiba Made in Kawasaki Technical Research Institute of Iron Co., Ltd. F-term (reference) 4D075 AA04 AA69 AA85 BB14Y BB24Z CA09 CA23 DA11 DB02 DB04 DB06 DB07 DB13 DB14 DC13 DC19 EA06 EA07 EA13 EB01 EB32 EB33 EC01 EC07 4G004 BA00 4K026 AA02 AA04 AA06 AA09 AA23 BA03 BB05 CA16 CA23 CA37 DA04 DA06
Claims (3)
に配設した攪拌羽根を先端部の回転速度 1.5ｍ／sec 以
上で回転させ、同時に前記粉体の上方から 3.0ｍ／sec
以上の流速で流動用ガスを前記粉体中に吹き込むことに
よって前記粉体を攪拌流動させるとともに、前記粉体の
上方から被覆液を噴霧することにより、前記粉体に前記
被覆液を付与しかつ前記被覆液を乾燥させ、被覆層を形
成することを特徴とする粉体の被覆方法。1. A container containing powder, and a stirring blade disposed at the bottom of the container is rotated at a tip speed of 1.5 m / sec or more, and at the same time 3.0 m / sec from above the powder.
While agitating and flowing the powder by blowing a flowing gas into the powder at the above flow rate, by spraying the coating liquid from above the powder, to impart the coating liquid to the powder and A method for coating powder, comprising drying the coating liquid to form a coating layer.
30ｍ／sec で回転させ、かつ前記流動用ガスを 3.0〜50
0 ｍ／sec の流速で前記粉体に吹き込むことを特徴とす
る請求項１に記載の粉体の被覆方法。2. The rotating speed of the stirring blade at the tip is 1.5 to
Rotate at 30m / sec, and flow gas is 3.0 ～ 50
The powder coating method according to claim 1, wherein the powder is blown into the powder at a flow rate of 0 m / sec.
前記被覆液が第１リン酸アルミニウム水溶液であること
を特徴とする請求項１または２に記載の粉体の被覆方
法。3. The powder is iron powder or steel powder,
The powder coating method according to claim 1, wherein the coating liquid is a first aluminum phosphate aqueous solution.
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| JP2002-76445 | 2002-03-19 | ||
| JP2002076445 | 2002-03-19 | ||
| JP2003075202A JP4055617B2 (en) | 2002-03-19 | 2003-03-19 | Powder coating method |
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| JP4055617B2 JP4055617B2 (en) | 2008-03-05 |
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| JP2010285633A (en) * | 2009-06-09 | 2010-12-24 | Kobe Steel Ltd | Method of producing powder mixture for powder metallurgy, and method of producing sintered body |
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| JP2018086624A (en) * | 2016-11-28 | 2018-06-07 | 株式会社Flosfia | Film deposition apparatus and film deposition method |
| KR101900306B1 (en) * | 2017-08-10 | 2018-09-20 | (주)포스코켐텍 | Dry coating equipment of quicklime for steelmaking and silicone oil surface treatment method using the same |
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2003
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010285633A (en) * | 2009-06-09 | 2010-12-24 | Kobe Steel Ltd | Method of producing powder mixture for powder metallurgy, and method of producing sintered body |
| CN104648730A (en) * | 2014-12-15 | 2015-05-27 | 苏州欣航微电子有限公司 | Electric heater temperature control tube glue and powder spray device |
| JP2018086624A (en) * | 2016-11-28 | 2018-06-07 | 株式会社Flosfia | Film deposition apparatus and film deposition method |
| CN107293397A (en) * | 2017-08-03 | 2017-10-24 | 山东汇嘉磁电科技有限公司 | The annular conjuncted fluidisation painting device of soft magnetic-powder core and its coating process |
| CN107293397B (en) * | 2017-08-03 | 2023-05-23 | 山东汇嘉磁电科技有限公司 | Annular soft magnetic powder core conjuncted fluidization coating device and coating method thereof |
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| WO2019031918A3 (en) * | 2017-08-10 | 2019-04-25 | (주)포스코켐텍 | Dry-coating apparatus of quicklime for steel making and method for surface treatment with silicon oil using same |
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