JPS6333507A - Method and apparatus for producing fine spheroidal powder - Google Patents
Method and apparatus for producing fine spheroidal powderInfo
- Publication number
- JPS6333507A JPS6333507A JP17287586A JP17287586A JPS6333507A JP S6333507 A JPS6333507 A JP S6333507A JP 17287586 A JP17287586 A JP 17287586A JP 17287586 A JP17287586 A JP 17287586A JP S6333507 A JPS6333507 A JP S6333507A
- Authority
- JP
- Japan
- Prior art keywords
- raw material
- powder
- material powder
- laser beam
- melting
- 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 54
- 238000000034 method Methods 0.000 title description 11
- 239000002994 raw material Substances 0.000 claims abstract description 29
- 238000001816 cooling Methods 0.000 claims abstract description 27
- 238000002844 melting Methods 0.000 claims abstract description 21
- 230000008018 melting Effects 0.000 claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 230000001590 oxidative effect Effects 0.000 claims description 5
- 230000001678 irradiating effect Effects 0.000 claims description 2
- 239000007789 gas Substances 0.000 abstract description 16
- 239000002245 particle Substances 0.000 abstract description 13
- 239000012159 carrier gas Substances 0.000 abstract description 9
- 238000005192 partition Methods 0.000 abstract description 4
- 239000000155 melt Substances 0.000 abstract description 2
- 239000010419 fine particle Substances 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 3
- 229910001111 Fine metal Inorganic materials 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000010301 surface-oxidation reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009689 gas atomisation Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Landscapes
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
Description
【発明の詳細な説明】
［技術分野］
本発明は球状微粉体の製造に関し、特に高密度のプリン
ト回路等を形成するのに好適な球状金属微粉体の製造方
法に関する。DETAILED DESCRIPTION OF THE INVENTION [Technical Field] The present invention relates to the production of spherical fine powder, and particularly to a method for producing spherical fine metal powder suitable for forming high-density printed circuits and the like.
［従来技術と問題点」
高密度プリント回路を形成するには金属微粉体を含有す
る厚膜ペーストを絶縁基板上に塗布し、該厚膜ペースト
を利用して目的の回路パターンをプリントする。該厚膜
ペーストに含まれる金属微粉体を製造するには、従来、
ａ金属酸化物を還元する方法、ｂ金属塩水溶液を電解す
る方法、ｃＩｌ械的粉砕法などが知られており数千Ａか
ら十数ル程度の微細粒子が製造される。[Prior Art and Problems] To form a high-density printed circuit, a thick film paste containing fine metal powder is applied onto an insulating substrate, and the thick film paste is used to print a desired circuit pattern. Conventionally, in order to produce the metal fine powder contained in the thick film paste,
A method of reducing a metal oxide, b a method of electrolyzing an aqueous solution of a metal salt, a method of cIl mechanical pulverization, etc. are known, and fine particles ranging from several thousand A to a dozen or so L are produced.
ところが、上記方法により製造される微粒子はフレーク
状であり、または不定形であり、更には粒子表面が酸化
されている場合が多く１回路パターンの線幅や線間隔を
小さくすることが出来ないため、高密度の微細な回路パ
ターンを形成するには限界がある。However, the fine particles produced by the above method are flaky or irregular in shape, and the particle surface is often oxidized, making it impossible to reduce the line width and line spacing of one circuit pattern. However, there are limits to the formation of high-density, fine circuit patterns.
他方、球状の微粉体を得るには、従来、ガスアトマイズ
法、回転電極法などが知られているが、これらの方法で
は２０ｇ以下の微粒子を製造するのが困難である。高密
度の回路パターンを製造するには２０ｗ以下の微細粒子
が必要であり、上記方法は粒度が大き過ぎて適さない。On the other hand, gas atomization methods, rotating electrode methods, and the like are conventionally known for obtaining spherical fine powder, but it is difficult to produce fine particles of 20 g or less using these methods. In order to manufacture high-density circuit patterns, fine particles of 20 W or less are required, and the above method is not suitable because the particle size is too large.
以上のように現状の製造方法によって得られる微粉体は
形状異方性や表面酸化あるいは粒度の点で高密度プリン
ト回路の厚膜ペースト材料として不充分である。As described above, the fine powder obtained by the current manufacturing method is insufficient as a thick film paste material for high-density printed circuits in terms of shape anisotropy, surface oxidation, and particle size.
［問題解決の知見］
本発明者等は、原料粉末を凝集しないように溶融すれば
球状化すること、および酸化した粉末はそのまま溶融し
ても球状化しないが表面の酸化層を還元すれば球状化し
うろことを見出した。[Knowledge for solving the problem] The present inventors discovered that if the raw material powder is melted without agglomeration, it will become spheroidal, and that oxidized powder will not become spherical even if it is melted as is, but if the oxidized layer on the surface is reduced, it will become spherical. I discovered scales that turned into fish.
［発明の構成］
本発明は、非酸化性ガス雰囲気中でレーザビームを用い
て原料粉末を急速に溶融することにより原料粉末を微細
化し、球状微粉体を得るものであり、本発明によれば、
原料粉体を非酸化性ガスで搬送しつつ該ガス流にレーザ
ビームを照射して原料粉体を溶融、急冷することを特徴
とする球状微粉体の製造方法が提供される。[Structure of the Invention] The present invention is to refine a raw material powder by rapidly melting the raw material powder using a laser beam in a non-oxidizing gas atmosphere to obtain a spherical fine powder. ,
A method for producing spherical fine powder is provided, which comprises transporting the raw material powder in a non-oxidizing gas and irradiating the gas flow with a laser beam to melt and rapidly cool the raw material powder.
また本発明によれば、原料粉体の溶融冷却室と、該溶融
冷却室に連通した捕集室とを有し、該溶融冷却室にはレ
ーザビーム照射部と、該レーザビームの焦点領域に原料
粉体を供給するガス供給路と、レーザビーム照射後のガ
ス流を冷却する冷却手段を有することを特徴とする球状
微粉体製造装置が提供される。Further, according to the present invention, there is provided a melting and cooling chamber for the raw material powder and a collection chamber communicating with the melting and cooling chamber, and the melting and cooling chamber includes a laser beam irradiation section and a focal region of the laser beam. Provided is a spherical fine powder manufacturing apparatus characterized by having a gas supply path for supplying raw material powder and a cooling means for cooling the gas flow after laser beam irradiation.
第１図に本発明に係る球状微粉体製造装置の概略を示す
。FIG. 1 schematically shows an apparatus for producing spherical fine powder according to the present invention.
図示するように本装置は、原料粉体の溶融冷却室１０と
、該溶融冷却室１０に連通した捕集室２０とを有する。As shown in the figure, this apparatus includes a melting and cooling chamber 10 for raw material powder, and a collection chamber 20 communicating with the melting and cooling chamber 10.
該溶融冷却室ｌＯの内部には隔壁１１が設けられており
、該隔壁１１により上記溶融冷却室１０の内部が溶融部
１０ａと冷却部１０ｂとに区画されている。溶融部１０
ａにはレーザビームの照射部１２が設けられており、該
照射部１２はレーザ発振器１３が接続する。照射部１２
には第２図に示すようにレーザビームを収束させるレン
ズ１４と、該レーザビームの焦点領域に原料粉体を供給
するガス供給路１５とが設けられている６該ガス供給路
１５はレーザビームの焦点付近に開口する円錐状のノズ
ル１６を有しており、原料粉体はキャリアガスと共に該
ノズル１６からレーザビームと略同軸方向に噴出される
。尚、原料粉体の噴出方向はレーザビームと同軸に限ら
ない。該溶融部１０ａの底部には未溶融の粉体を回収す
るだめの回収器１９が付設されている０次に上記隔壁１
１にはレーザビームが照射された原料粉体ガス流を冷却
部１０ｂに導く孔１７が穿設されており、更に該冷却部
１０ｂの外周には水冷パイプ１８が配設されている。上
記冷却部１０ｂには捕集室２０が連設されており、該捕
集室２０の内部にはフィルターユニットが収納される一
方その外周には水冷パイプ２３が設けられている。また
捕集室底部には捕集器２１が設けられており、捕集室上
部には排気ダクト２２が連設されている。A partition wall 11 is provided inside the melting cooling chamber IO, and the partition wall 11 divides the inside of the melting cooling chamber 10 into a melting section 10a and a cooling section 10b. Melting part 10
A is provided with a laser beam irradiation section 12, and a laser oscillator 13 is connected to the irradiation section 12. Irradiation section 12
As shown in FIG. 2, a lens 14 for converging the laser beam and a gas supply path 15 for supplying raw material powder to the focal region of the laser beam are provided. The laser beam has a conical nozzle 16 that opens near the focal point of the laser beam, and the raw material powder is ejected from the nozzle 16 along with a carrier gas in a direction substantially coaxial with the laser beam. Note that the direction in which the raw material powder is ejected is not limited to being coaxial with the laser beam. A collector 19 for collecting unmelted powder is attached to the bottom of the melting section 10a.
1 is provided with a hole 17 for guiding the flow of raw material powder gas irradiated with a laser beam to a cooling section 10b, and furthermore, a water cooling pipe 18 is disposed around the outer periphery of the cooling section 10b. A collection chamber 20 is connected to the cooling section 10b, and a filter unit is housed inside the collection chamber 20, and a water cooling pipe 23 is provided around the outer circumference of the collection chamber 20. A collector 21 is provided at the bottom of the collection chamber, and an exhaust duct 22 is connected to the top of the collection chamber.
上記装置構成において、原料粉体はキャリアガスと共に
ガス供給路１５を経てノズル１６から溶融冷却室ｌＯの
内部に噴射される。キャリアガスとしては原料粉体が酸
化しない非酸化性ガスが用いられ、具体的には窒素ガス
などの不活性ガス、アンモニアガスなどの還元性ガス或
いはこれらの混合ガスが用いられる。キャリアガス中の
最適な原料粉体の量およびガス流速はレーザ出力により
異なるが１例えば、５ＫＷのＣＯ２ガスレーザの場合に
は原料粉体の量は３マｏ１％以下であるのが良い、３マ
ロ１％より多いと原料粉体が充分に溶融されず球状化し
ない粒子の割合が増し、また粒子相互の結合を生じるよ
うになる。また該ガス流の流速は上記ノズル口において
１０００ ｃ ｍ ７秒以上とするのが良い、該流速の
とき微粒子相互の結合を生じ難く、数ルの微粉体を得る
ことが出来る。In the above device configuration, the raw material powder is injected into the melting cooling chamber IO from the nozzle 16 through the gas supply path 15 together with the carrier gas. As the carrier gas, a non-oxidizing gas that does not oxidize the raw material powder is used, specifically an inert gas such as nitrogen gas, a reducing gas such as ammonia gas, or a mixed gas thereof. The optimal amount of raw material powder in the carrier gas and the gas flow rate vary depending on the laser output. For example, in the case of a 5KW CO2 gas laser, the amount of raw material powder is preferably 3% or less, 3% or less. If it is more than 1%, the raw material powder will not be melted sufficiently and the proportion of particles that will not become spherical will increase, and particles will become bonded to each other. Further, the flow rate of the gas stream is preferably set to 1000 cm/7 seconds or more at the nozzle opening.At this flow rate, it is difficult for fine particles to bond with each other, and several liters of fine powder can be obtained.
発振器１３から発振されたレーザビームはレンズ１４に
より収束され、その焦点付近の原料粉体を溶融し、球状
の微細な粒子にする。この場合レーザビームで加熱され
るのはビームの焦点近傍に限られ、溶融後は急速に冷却
されるので溶融された微粒子が相互に結合することがな
い。尚、加熱手段としてプラズマを用いる方法が知られ
ているが、プラズマジェットの加熱領域はレーザービー
ムよりも広く、溶融され？＆細化された微粒子が該加熱
領域を飛行する間に微粒子相互の結合により、粗大化す
る欠点がある。またキャリアガスが加熱される温度も高
く、プラズマジェットの加熱領域経過後にもキャリアガ
スの雰囲気温度により微粒子が結合して粗大化する問題
もある。この点、本発明のレーザビームは加熱領域が狭
く、このような問題を生じない、レーザビームにより溶
融され微細化された粒子は隔壁１■の孔１７を通過して
冷却部１０ｂに導かれ、１００℃程度に冷却された後、
捕集部２０において捕集される。The laser beam emitted from the oscillator 13 is focused by the lens 14 and melts the raw material powder near the focal point to form fine spherical particles. In this case, only the area near the focus of the laser beam is heated by the laser beam, and after melting, the particles are rapidly cooled, so that the molten particles do not bond with each other. It should be noted that a method using plasma as a heating means is known, but the heating area of a plasma jet is wider than that of a laser beam, so it is difficult to melt. & There is a drawback that fine particles become coarse due to bonding with each other while flying through the heating region. Further, the temperature at which the carrier gas is heated is high, and there is also the problem that even after the heating region of the plasma jet has passed, the fine particles are combined and become coarse due to the atmospheric temperature of the carrier gas. In this respect, the laser beam of the present invention has a narrow heating area and does not cause such a problem.The particles melted and made fine by the laser beam are guided to the cooling part 10b through the holes 17 of the partition wall 12. After being cooled to around 100℃,
It is collected in the collection section 20.
尚、キャリアガスは排気ダクト２２を経て外部に導かれ
、必要に応じて再使用される。また未溶融粉末は溶融部
の底部に設けた回収器１９により回収される。Note that the carrier gas is led to the outside through the exhaust duct 22 and is reused as necessary. Further, the unmelted powder is collected by a collector 19 provided at the bottom of the melting section.
［発明の効果］
本発明の製造方法によれば、原料粉体の形状如何に拘ら
ず、微細なかつ球状の微粉体を容易に得ることが出来る
。[Effects of the Invention] According to the production method of the present invention, fine and spherical fine powder can be easily obtained regardless of the shape of the raw material powder.
更に本発明の製造方法は、非酸化性のキャリアガスを用
いるので粒子表面の酸化が防止され、殆ど表面酸化のな
い微細粒子を得ることが出来る。Furthermore, since the manufacturing method of the present invention uses a non-oxidizing carrier gas, oxidation of the particle surface is prevented, and fine particles with almost no surface oxidation can be obtained.
［実施例および比較例］
実施例
第１図に示す製造装置を用い（出力５ｋｗ、ビーム径３
インチ、焦点圧ｒａ８インチ）、第１表に示す原料粉体
について微粉体を製造した。得られた微粉体の性状を第
１表に併せて示す。[Example and Comparative Example] Using the manufacturing equipment shown in Figure 1 of Example (output 5 kW, beam diameter 3
inch, focal pressure ra 8 inches), and fine powders were produced using the raw material powders shown in Table 1. The properties of the obtained fine powder are also shown in Table 1.
比較例
第１表に示す原料粉体についてプラズマ法により微粉体
を製造した。得られた粉体の性状を第１表に併せて示す
。Comparative Example Fine powders were produced using the plasma method using the raw material powders shown in Table 1. The properties of the obtained powder are also shown in Table 1.
第１図は本発明に係る製造装置の概略断面図、第２図は
該装置の照射部の概略断面図である。
図面中、１〇−溶融冷却室、 １０ａ−溶融部、１０
ｂ−冷却部、 ２０−捕集室、 １２−レーザビーム
照射部、 １５−ガス供給路、 １８．２３−水冷
バイブである。
特許出願人 三菱金属株式会社
代理人 弁理士 松井政広 化１名
第１図
／ｌ’１
／’／
第２図FIG. 1 is a schematic sectional view of a manufacturing apparatus according to the present invention, and FIG. 2 is a schematic sectional view of an irradiation section of the apparatus. In the drawings, 10-melting cooling chamber, 10a-melting section, 10
b-cooling section, 20-collection chamber, 12-laser beam irradiation section, 15-gas supply path, 18.23-water-cooled vibrator. Patent applicant Mitsubishi Metals Co., Ltd. Agent Patent attorney Masahiro Matsui 1 person Figure 1/l'1 /'/ Figure 2
Claims (2)
レーザビームを照射して原料粉体を溶融、急冷すること
を特徴とする球状微粉体の製造方法。(1) A method for producing spherical fine powder, which comprises transporting the raw material powder with a non-oxidizing gas and irradiating the gas flow with a laser beam to melt and rapidly cool the raw material powder.
た捕集室とを有し、該溶融冷却室にはレーザビーム照射
部と、該レーザビームの焦点領域に原料粉体を供給する
ガス供給路と、レーザビーム照射後のガス流を冷却する
冷却手段を有することを特徴とする球状微粉体製造装置
。(2) It has a melting and cooling chamber for the raw material powder and a collection chamber that communicates with the melting and cooling chamber, and the melting and cooling chamber has a laser beam irradiation section and the raw material powder is placed in the focal region of the laser beam. A spherical fine powder production apparatus characterized by having a gas supply path and a cooling means for cooling the gas flow after laser beam irradiation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61172875A JP2508506B2 (en) | 1986-07-24 | 1986-07-24 | Spherical fine powder manufacturing method and manufacturing apparatus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61172875A JP2508506B2 (en) | 1986-07-24 | 1986-07-24 | Spherical fine powder manufacturing method and manufacturing apparatus |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6333507A true JPS6333507A (en) | 1988-02-13 |
| JP2508506B2 JP2508506B2 (en) | 1996-06-19 |
Family
ID=15949925
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61172875A Expired - Lifetime JP2508506B2 (en) | 1986-07-24 | 1986-07-24 | Spherical fine powder manufacturing method and manufacturing apparatus |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2508506B2 (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63243212A (en) * | 1987-03-16 | 1988-10-11 | ジー・ティー・イー・プロダクツ・コーポレイション | Wet metallurgical method for producing finely divided globular high melting point metal base powder |
| WO1991008850A1 (en) * | 1989-12-07 | 1991-06-27 | Nippon Steel Corporation | Method of manufacturing minute metallic balls uniform in size |
| US5761779A (en) * | 1989-12-07 | 1998-06-09 | Nippon Steel Corporation | Method of producing fine metal spheres of uniform size |
| WO2001008795A1 (en) * | 1999-08-02 | 2001-02-08 | Choi Man Soo | Fine particle manufacturing method using laser beam |
| CN107876783A (en) * | 2017-12-08 | 2018-04-06 | 西安交通大学 | Laser gain material manufacture metal powder preparation method based on laser fixed point interval scan |
| CN110893468A (en) * | 2019-12-26 | 2020-03-20 | 安徽工业大学 | Method and device for preparing spherical metal powder by combined atomization |
| CN114260454A (en) * | 2021-12-24 | 2022-04-01 | 四川大学 | Preparation method of high-quality spherical metal powder |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58151402A (en) * | 1981-10-26 | 1983-09-08 | Pilot Pen Co Ltd:The | Method for spheroidizing abrasion resistant alloy |
| JPS60224706A (en) * | 1984-04-20 | 1985-11-09 | Hitachi Ltd | Production of ultrafine metallic particles |
| JPS61136606A (en) * | 1984-12-06 | 1986-06-24 | Toyobo Co Ltd | Production of ultrafine powder |
-
1986
- 1986-07-24 JP JP61172875A patent/JP2508506B2/en not_active Expired - Lifetime
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58151402A (en) * | 1981-10-26 | 1983-09-08 | Pilot Pen Co Ltd:The | Method for spheroidizing abrasion resistant alloy |
| JPS60224706A (en) * | 1984-04-20 | 1985-11-09 | Hitachi Ltd | Production of ultrafine metallic particles |
| JPS61136606A (en) * | 1984-12-06 | 1986-06-24 | Toyobo Co Ltd | Production of ultrafine powder |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63243212A (en) * | 1987-03-16 | 1988-10-11 | ジー・ティー・イー・プロダクツ・コーポレイション | Wet metallurgical method for producing finely divided globular high melting point metal base powder |
| WO1991008850A1 (en) * | 1989-12-07 | 1991-06-27 | Nippon Steel Corporation | Method of manufacturing minute metallic balls uniform in size |
| US5761779A (en) * | 1989-12-07 | 1998-06-09 | Nippon Steel Corporation | Method of producing fine metal spheres of uniform size |
| WO2001008795A1 (en) * | 1999-08-02 | 2001-02-08 | Choi Man Soo | Fine particle manufacturing method using laser beam |
| CN107876783A (en) * | 2017-12-08 | 2018-04-06 | 西安交通大学 | Laser gain material manufacture metal powder preparation method based on laser fixed point interval scan |
| CN107876783B (en) * | 2017-12-08 | 2020-05-22 | 西安交通大学 | Laser additive manufacturing metal powder preparation method based on laser fixed-point interval scanning |
| CN110893468A (en) * | 2019-12-26 | 2020-03-20 | 安徽工业大学 | Method and device for preparing spherical metal powder by combined atomization |
| CN114260454A (en) * | 2021-12-24 | 2022-04-01 | 四川大学 | Preparation method of high-quality spherical metal powder |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2508506B2 (en) | 1996-06-19 |
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