JP2001062332A - Classification method of nickel powder - Google Patents

Classification method of nickel powder

Info

Publication number
JP2001062332A
JP2001062332A JP24489599A JP24489599A JP2001062332A JP 2001062332 A JP2001062332 A JP 2001062332A JP 24489599 A JP24489599 A JP 24489599A JP 24489599 A JP24489599 A JP 24489599A JP 2001062332 A JP2001062332 A JP 2001062332A
Authority
JP
Japan
Prior art keywords
nickel powder
slurry
powder
discharged
particle size
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
Application number
JP24489599A
Other languages
Japanese (ja)
Other versions
JP3549446B2 (en
Inventor
Takayuki Ito
孝之 伊藤
Hideo Takatori
英男 高取
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Toho Titanium Co Ltd
Original Assignee
Toho Titanium Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority to JP24489599A priority Critical patent/JP3549446B2/en
Application filed by Toho Titanium Co Ltd filed Critical Toho Titanium Co Ltd
Priority to CNB008018405A priority patent/CN1248814C/en
Priority to PCT/JP2000/005688 priority patent/WO2001015838A1/en
Priority to KR10-2001-7005080A priority patent/KR100422719B1/en
Priority to EP00954973A priority patent/EP1129804A4/en
Priority to US09/786,032 priority patent/US6454830B1/en
Priority to TW089117620A priority patent/TW522172B/en
Publication of JP2001062332A publication Critical patent/JP2001062332A/en
Application granted granted Critical
Publication of JP3549446B2 publication Critical patent/JP3549446B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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  • Powder Metallurgy (AREA)

Abstract

PROBLEM TO BE SOLVED: To efficiently classify a nickel powder low in the content of coarse particles and having a narrow particle size distribution. SOLUTION: A nickel powder with a mean particle size of 0.1-1.0 μm is dispersed in water to prepare a slurry with a concn. of 5-25 wt.% and this slurry is supplied to a liquid cyclone for classifying the powder in a powder mixed liquid into at least coarse particles and fine particles. 5-80 wt.% of the nickel powder in the slurry is discharged from the fine particle discharge port of the cyclone and the remainder thereof is discharged from the coarse particle discharge port thereof.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は、例えば電子部品等
に用いられる導電ペーストフィラーの材料として有用な
超微粉状ニッケル粉等のニッケル粉の分級方法に関す
る。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for classifying nickel powder such as ultrafine nickel powder which is useful as a material for a conductive paste filler used for electronic parts and the like.

【0002】[0002]

【従来の技術】Ni、Cu、Ag等の導電性の金属粉
は、積層セラミックコンデンサの内部電極形成用として
有用であり、とりわけニッケル粉は、従来のPd粉等に
比べて安価なため注目されている。そして、積層セラミ
ックコンデンサの小型化、大容量化に伴って内部電極は
1〜2μm前後の薄層化の傾向にあり、したがって、ニ
ッケル粉の粒径は1μm、もしくはそれ以下であること
が要求されてきている。
2. Description of the Related Art Conductive metal powders such as Ni, Cu, and Ag are useful for forming internal electrodes of multilayer ceramic capacitors, and nickel powder is particularly attracting attention because it is less expensive than conventional Pd powders. ing. With the miniaturization and large capacity of the multilayer ceramic capacitor, the internal electrodes tend to be thinner to about 1 to 2 μm. Therefore, the particle size of the nickel powder is required to be 1 μm or less. Is coming.

【0003】このような特性を満足するニッケル粉とし
ては、ニッケルの純度が99.5wt%以上で、しかも
粒径が0.05〜1.0μmの微細な球状ニッケル粉
が、特開平3−280304号公報に開示されている。
このニッケル粉によれば、電極層中の充填密度を高くす
ることができるので、焼成後の電極層の比抵抗が小さ
く、また、デラミネーション(剥離)やクラックが起こ
りにくいとされている。
As a nickel powder satisfying such characteristics, fine spherical nickel powder having a nickel purity of 99.5 wt% or more and a particle size of 0.05 to 1.0 μm is disclosed in Japanese Patent Application Laid-Open No. 3-280304. No. 6,086,045.
According to this nickel powder, the packing density in the electrode layer can be increased, so that the specific resistance of the fired electrode layer is small, and delamination (peeling) and cracks are less likely to occur.

【0004】[0004]

【発明が解決しようとする課題】ところで、ニッケル粉
の製造方法としては、塩化ニッケルガスを水素ガスによ
り還元させる気相還元法が近年では一般的となってい
る。同方法は、球状ニッケル粉を効率よく製造すること
ができるといった利点を備えているものの、粒径が1μ
m以上のニッケル粉が含まれる場合も多かった。例え
ば、平均粒径が0.4μmであっても、1〜2μm、時
には5μmといった粒子が含まれている場合もあり、特
性上好ましいものではない。そこで、1μm以上の粗粒
を効率的に除去することのできる分級技術が望まれてい
る。
Incidentally, as a method for producing nickel powder, a gas phase reduction method in which nickel chloride gas is reduced with hydrogen gas has become popular in recent years. This method has the advantage that spherical nickel powder can be efficiently produced, but the particle size is 1 μm.
m or more in many cases. For example, even if the average particle diameter is 0.4 μm, particles having a particle diameter of 1 to 2 μm and sometimes 5 μm may be contained, which is not preferable in terms of characteristics. Therefore, a classification technique capable of efficiently removing coarse particles of 1 μm or more is desired.

【0005】本発明は上記事情に鑑みてなされたもの
で、以下を目的としている。 粗粒の含有率が低く、粒度分布の狭いニッケル粉の分
級方法を提供する。 具体的には、平均粒径が0.1〜1.0μmのニッケ
ル粉中に存在する粒径2μm以上の粗粒を、100万分
の100部以下の含有量に抑える分級方法を提供する。
The present invention has been made in view of the above circumstances, and has the following objects. Provided is a method for classifying nickel powder having a low content of coarse particles and a narrow particle size distribution. Specifically, the present invention provides a classification method for suppressing coarse particles having a particle diameter of 2 μm or more present in nickel powder having an average particle diameter of 0.1 to 1.0 μm to a content of 100 parts per million or less.

【0006】[0006]

【課題を解決するための手段】本発明者らは、上記目的
を達成する手段として液体サイクロンの使用による分級
方法を鋭意検討した結果、水を媒体としてニッケル粉を
スラリー化し、このスラリーを液体サイクロンに供給す
る際のスラリー濃度(ニッケル粉含有率)が分級効果に
大きな影響をもたらすことを発見し、本発明の完成に至
った。すなわち本発明は、粉体混合液中の粉体を少なく
とも粗粒と細粒とに分級する液体サイクロンに、平均粒
径0.1〜1.0μmのニッケル粉を5〜25wt%含
有させたスラリーを供給することを特徴としている。こ
の場合の粗粒は粒径が2μm以上の粉、また、細粒は2
μm未満の粉であって本発明の目的とするニッケル粉と
定義する。
Means for Solving the Problems The present inventors have intensively studied a classification method using a liquid cyclone as a means for achieving the above object, and as a result, slurried nickel powder using water as a medium, It has been discovered that the slurry concentration (nickel powder content) at the time of supply to the vessel has a great effect on the classification effect, and the present invention has been completed. That is, the present invention provides a slurry in which a liquid cyclone that classifies powder in a powder mixture into at least coarse particles and fine particles contains 5 to 25 wt% of nickel powder having an average particle size of 0.1 to 1.0 μm. It is characterized by supplying. In this case, coarse particles are powder having a particle size of 2 μm or more, and fine particles are powder having a particle size of 2 μm or more.
It is defined as a nickel powder having a size of less than μm and intended for the present invention.

【0007】また、本発明では、スラリー中のニッケル
粉の5〜80%を液体サイクロンの細粒排出口から排出
させ、残部を粗粒排出口から排出させることを好ましい
形態としている。
Further, in the present invention, it is preferable that 5 to 80% of the nickel powder in the slurry is discharged from the fine particle discharge port of the liquid cyclone, and the remainder is discharged from the coarse particle discharge port.

【0008】次に、本発明のより具体的な手段を説明す
る。A.液体サイクロン 本発明の液体サイクロンとしては、細粒を装置のトップ
部(上部)から排出し、粗粒を装置のボトム部(底部)
から排出するタイプの二液分離型や、細粒より細かな微
細粒を装置のトップ部から排出し、細粒を装置のミドル
部(中間部)から排出し、粗粒を装置のボトム部から排
出するタイプの三液分離型が挙げられる。これらの中で
は、粒径を細かく制御することができる観点から後者の
タイプがより好ましく用いられる。
Next, more specific means of the present invention will be described. A. Hydrocyclone As the hydrocyclone of the present invention, fine particles are discharged from the top part (upper part) of the apparatus, and coarse particles are discharged from the bottom part (bottom part) of the apparatus.
Or two-part separation type, which discharges fine particles finer than fine particles from the top of the device, fine particles from the middle part (intermediate part) of the device, and coarse particles from the bottom of the device A three-liquid separation type of discharging type is exemplified. Among these, the latter type is more preferably used from the viewpoint that the particle size can be finely controlled.

【0009】液体サイクロンの材質は、耐食性および耐
摩耗性を確保する上でセラミックス製が好ましい。セラ
ミックスとしては、アルミナや窒化ケイ素が好ましい。
液体サイクロンは、1基あるいは複数を並列させて稼動
させてもよく、複数の液体サイクロンを並列稼動させる
ことにより、大量生産を可能とし生産性向上の上で効果
的である。
The material of the liquid cyclone is preferably made of ceramics in order to ensure corrosion resistance and wear resistance. As the ceramics, alumina and silicon nitride are preferable.
One or a plurality of hydrocyclones may be operated in parallel, and by operating a plurality of hydrocyclones in parallel, mass production is possible, which is effective in improving productivity.

【0010】B.スラリー 本発明では、ニッケル粉をスラリー化する際の媒体とし
て、水が好ましく用いられる。水の中に、平均粒径0.
1〜1.0μmのニッケル粉を分散させてスラリーを
得、これを液体サイクロンに供給するわけであるが、ス
ラリー中のニッケル粉の含有率(スラリー濃度)は、5
〜25wt%、好ましくは7〜20wt%、より好まし
くは8〜15wt%がよい。
B. Slurry In the present invention, water is preferably used as a medium when the nickel powder is slurried. In water, the average particle size is 0.
A slurry is obtained by dispersing nickel powder of 1 to 1.0 μm and supplied to a liquid cyclone. The content (slurry concentration) of nickel powder in the slurry is 5%.
-25 wt%, preferably 7-20 wt%, more preferably 8-15 wt%.

【0011】スラリー濃度に関し、上記三液分離型の液
体サイクロンを用いて分級効率を調べたところ、ニッケ
ル粉が5wt%を下回ると、トップ部および/またはミ
ドル部から排出されるスラリー中に粗粒が混入しやすく
なり好ましくなかった。スラリー濃度を高めていくにつ
れ、トップ部および/またはミドル部から排出されるス
ラリー中の粗粒の含有率は急激に低下したが、20wt
%を超えると再び分級効率が低下し、ニッケル粉中に粗
粒が多く含まれる傾向にあった。以上を根拠として、本
発明のスラリー中のニッケル粉含有率を上記の範囲とし
た。
With respect to the slurry concentration, the classification efficiency was examined using the above-mentioned three-liquid separation type cyclone. When the nickel powder was less than 5 wt%, coarse particles were contained in the slurry discharged from the top part and / or the middle part. Was easily mixed, which was not preferable. As the slurry concentration was increased, the content of coarse particles in the slurry discharged from the top portion and / or the middle portion was sharply reduced, but was 20 wt.
%, The classification efficiency was reduced again, and a large amount of coarse particles tended to be contained in the nickel powder. Based on the above, the nickel powder content in the slurry of the present invention was set in the above range.

【0012】スラリー中のニッケル粉の含有率は、上記
範囲の中にあって特に7〜20wt%、とりわけ8〜1
5wt%の場合に、生産効率および分級効率が著しく良
好であることから特に好ましい。ちなみに、この範囲で
は100万個のニッケル粒子に対して粗粒の含有量は僅
かに10〜100個と、きわめて効率的な分級を達成す
ることができる。
[0012] The content of nickel powder in the slurry is within the above range, preferably 7 to 20 wt%, particularly 8 to 1 wt%.
The case of 5 wt% is particularly preferable because the production efficiency and the classification efficiency are remarkably good. By the way, in this range, the content of coarse particles is only 10 to 100 particles per 1 million nickel particles, so that extremely efficient classification can be achieved.

【0013】C.液体サイクロンからのニッケル粉の排
出割合 本発明では、前述の如く、液体サイクロンに供給したス
ラリー中のニッケル粉の5〜80%を液体サイクロンの
細粒排出口から排出させ、残部を粗粒排出口から排出さ
せることを好ましい形態としている。この場合は、二液
分離型の液体サイクロンを前提としており、細粒排出口
は前記トップ部、粗粒排出口はボトム部を意味する。
C. Discharge of nickel powder from hydrocyclone
In the present invention, as described above, it is preferable that 5-80% of the nickel powder in the slurry supplied to the liquid cyclone is discharged from the fine particle discharge port of the liquid cyclone, and the remainder is discharged from the coarse particle discharge port. And In this case, a two-liquid separation type hydrocyclone is premised, and the fine particle outlet means the above-mentioned top portion and the coarse particle outlet means the bottom portion.

【0014】さらに好ましい排出の割合としては、上記
三液分離型の液体サイクロンを用い、該液体サイクロン
のトップ部および/またはミドル部からのニッケル粉の
排出量を5〜80wt%、好ましくは5〜70wt%と
する。この場合、さらに、ミドル部からのニッケル粉の
排出量を20〜75wt%とすることがもっとも好まし
い。なお、より精密に粗粒を分級する必要がある場合に
は、ミドル部から排出されて得たニッケル粉を、本発明
にしたがって再度スラリー化し、液体サイクロンに供給
するとよい。
As a more preferable discharge ratio, the above-mentioned three-liquid separation type hydrocyclone is used, and the discharge amount of nickel powder from the top part and / or middle part of the liquid cyclone is 5 to 80 wt%, preferably 5 to 80 wt%. 70 wt%. In this case, it is most preferable that the amount of nickel powder discharged from the middle part be 20 to 75 wt%. If it is necessary to classify coarse particles more precisely, the nickel powder discharged from the middle part may be re-slurried according to the present invention and supplied to the liquid cyclone.

【0015】以上のようにして液体サイクロンのトップ
部および/またはミドル部から排出されて得たスラリー
中のニッケル粉は、デカンテーション、フィルターなど
により水分と分離され、乾燥などの処理を経た後、製品
化される。
The nickel powder in the slurry discharged from the top and / or middle part of the hydrocyclone as described above is separated from moisture by a decanter, a filter, etc., and after being subjected to a treatment such as drying, Be commercialized.

【0016】[0016]

【実施例】以下、本発明に基づく実施例を説明する。塩
化ニッケルの気相還元法により製造された平均粒径0.
4μm(比表面積換算に基づくBET径)のニッケル粉
を水に分散させてスラリー化し、このスラリーを、三液
分離型の液体サイクロン(村田工業社製:TR−5型ス
ーパークロン)に供給してスラリー濃度(スラリー中の
ニッケル粉のwt%)の違いによる分級効率を調べた。
スラリー濃度、液体サイクロンへのスラリーの供給量お
よび供給圧力、ニッケル粉の供給量を、表1に示す。
Embodiments of the present invention will be described below. Average particle size produced by a gas phase reduction method of nickel chloride.
Nickel powder of 4 μm (BET diameter based on specific surface area conversion) is dispersed in water to form a slurry, and this slurry is supplied to a three-liquid separation type liquid cyclone (Murata Kogyo Co., Ltd .: TR-5 type supercron). The classification efficiency according to the difference in the slurry concentration (wt% of nickel powder in the slurry) was examined.
Table 1 shows the slurry concentration, the supply amount and supply pressure of the slurry to the liquid cyclone, and the supply amount of the nickel powder.

【0017】[0017]

【表1】 [Table 1]

【0018】液体サイクロンのトップ部、ミドル部およ
びボトム部から排出されたスラリー中のニッケル粉の排
出量を、次の表2に示す。
Table 2 shows the discharge amount of nickel powder in the slurry discharged from the top, middle and bottom portions of the hydrocyclone.

【0019】[0019]

【表2】 [Table 2]

【0020】スラリー濃度と「トップ部+ミドル部」の
ニッケル粉の排出率の関係を、図1に示す。図1に示す
ように、液体サイクロンに供給するスラリーの濃度を上
げるにしたがい、トップ部およびボトム部からのニッケ
ル粉の排出量が上昇するが、7wt%付近を境に一旦ニ
ッケル粉の排出量は下がり、10wt%を超えると再び
ニッケル粉の排出量が徐々に上がることが判った。
FIG. 1 shows the relationship between the slurry concentration and the discharge rate of nickel powder in the “top part + middle part”. As shown in FIG. 1, as the concentration of the slurry supplied to the hydrocyclone is increased, the amount of nickel powder discharged from the top portion and the bottom portion is increased. It was found that when the content exceeded 10 wt%, the amount of discharged nickel powder gradually increased again.

【0021】また、各試料を顕微鏡で観察して粒径1μ
mを超えるニッケル粉の存在を調べ、品質を評価した。
その評価結果を次の表3に示す。表3では、試験No.
2〜5のスラリー濃度が、品質を満足するニッケル粉が
トップ部およびミドル部から得られることが判り、本発
明が実証された。
Each sample was observed with a microscope to find a particle size of 1 μm.
m, and the quality was evaluated.
The evaluation results are shown in Table 3 below. In Table 3, the test No.
It was found that nickel concentrations satisfying the quality were obtained from the top portion and the middle portion at a slurry concentration of 2 to 5, demonstrating the present invention.

【0022】[0022]

【表3】 [Table 3]

【0023】なお、生産性を高める上では、液体サイク
ロンに供給するスラリーの濃度は高い方が好ましく、ま
た、分級後のニッケル粉の歩留まりを高める上ではトッ
プ部とミドル部から排出されるニッケル粉の重量が大き
いほど好ましい。したがって、上記実施例では、試験N
o.2のニッケル粉が特に好ましい。
In order to increase the productivity, it is preferable that the concentration of the slurry supplied to the liquid cyclone is higher. In order to increase the yield of the nickel powder after classification, the nickel powder discharged from the top portion and the middle portion is preferably used. It is more preferable that the weight is larger. Therefore, in the above embodiment, the test N
o. 2 nickel powder is particularly preferred.

【0024】[0024]

【発明の効果】以上説明したように、本発明によれば、
粉体混合液中の粉体を少なくとも粗粒と細粒とに分級す
る液体サイクロンに、平均粒径0.1〜1.0μmのニ
ッケル粉を5〜25wt%含有させたスラリーを供給し
てニッケル粉を分級することにより、粗粒の含有率が低
く、粒度分布の狭いニッケル粉を効率的に分級すること
ができる。
As described above, according to the present invention,
A slurry containing 5 to 25 wt% of nickel powder having an average particle size of 0.1 to 1.0 μm is supplied to a liquid cyclone that classifies the powder in the powder mixture into at least coarse particles and fine particles. By classifying the powder, it is possible to efficiently classify nickel powder having a low content of coarse particles and a narrow particle size distribution.

【図面の簡単な説明】[Brief description of the drawings]

【図1】 本発明の実施例に基づくスラリー濃度と「ト
ップ部+ミドル部」のニッケル粉の排出率の関係を示す
線図である。
FIG. 1 is a diagram showing a relationship between a slurry concentration and a discharge rate of nickel powder in a “top part + middle part” based on an embodiment of the present invention.

Claims (2)

【特許請求の範囲】[Claims] 【請求項1】 粉体混合液中の粉体を少なくとも粗粒と
細粒とに分級する液体サイクロンに、平均粒径0.1〜
1.0μmのニッケル粉を5〜25wt%含有させたス
ラリーを供給することを特徴とするニッケル粉の分級方
法。
1. A liquid cyclone for classifying powder in a powder mixture into at least coarse particles and fine particles, having an average particle size of 0.1 to
A method for classifying nickel powder, comprising supplying a slurry containing 5 to 25 wt% of nickel powder of 1.0 μm.
【請求項2】 前記スラリー中のニッケル粉の5〜80
%を、前記サイクロンの細粒排出口から排出させ、残部
を粗粒排出口から排出させることを特徴とする請求項1
に記載のニッケル粉の分級方法。
2. The method according to claim 1, wherein the nickel powder in the slurry is 5 to 80%.
% Is discharged from the fine-grain outlet of the cyclone, and the remainder is discharged from the coarse-grain outlet.
2. A method for classifying nickel powder as described in 1. above.
JP24489599A 1999-08-31 1999-08-31 Nickel powder classification method Expired - Lifetime JP3549446B2 (en)

Priority Applications (7)

Application Number Priority Date Filing Date Title
JP24489599A JP3549446B2 (en) 1999-08-31 1999-08-31 Nickel powder classification method
PCT/JP2000/005688 WO2001015838A1 (en) 1999-08-31 2000-08-24 Nickel powder for monolithic ceramic capacitor
KR10-2001-7005080A KR100422719B1 (en) 1999-08-31 2000-08-24 Nickel powder for monolithic ceramic capacitor
EP00954973A EP1129804A4 (en) 1999-08-31 2000-08-24 Nickel powder for monolithic ceramic capacitor
CNB008018405A CN1248814C (en) 1999-08-31 2000-08-24 Nickel powder for monolithic ceramic capacitor
US09/786,032 US6454830B1 (en) 1999-08-31 2000-08-24 Nickel powder for multilayer ceramic capacitors
TW089117620A TW522172B (en) 1999-08-31 2000-08-30 Nickel powder for laminated ceramic capacitors

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP24489599A JP3549446B2 (en) 1999-08-31 1999-08-31 Nickel powder classification method

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008088456A (en) * 2006-09-29 2008-04-17 Tdk Corp Method and apparatus for producing metal particle
JP2008142681A (en) * 2006-12-13 2008-06-26 Mitsui Mining & Smelting Co Ltd Wet type centrifugal classification method and metal fine particle slurry obtained by the same
JP2011156520A (en) * 2010-02-04 2011-08-18 Sumitomo Metal Mining Co Ltd Method of classifying metal fine powder
CN104475228A (en) * 2014-11-15 2015-04-01 中铝国际技术发展有限公司 Grading method for solid-liquid two-phase flow size
JP2015158001A (en) * 2014-02-25 2015-09-03 住友金属鉱山株式会社 Nickel powder production process

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008088456A (en) * 2006-09-29 2008-04-17 Tdk Corp Method and apparatus for producing metal particle
JP4656327B2 (en) * 2006-09-29 2011-03-23 Tdk株式会社 Metal particle manufacturing method and metal particle manufacturing apparatus
JP2008142681A (en) * 2006-12-13 2008-06-26 Mitsui Mining & Smelting Co Ltd Wet type centrifugal classification method and metal fine particle slurry obtained by the same
JP2011156520A (en) * 2010-02-04 2011-08-18 Sumitomo Metal Mining Co Ltd Method of classifying metal fine powder
JP2015158001A (en) * 2014-02-25 2015-09-03 住友金属鉱山株式会社 Nickel powder production process
CN104475228A (en) * 2014-11-15 2015-04-01 中铝国际技术发展有限公司 Grading method for solid-liquid two-phase flow size

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