JPH0672247B2 - Method for refining ultrafine metal powder - Google Patents
Method for refining ultrafine metal powderInfo
- Publication number
- JPH0672247B2 JPH0672247B2 JP15017388A JP15017388A JPH0672247B2 JP H0672247 B2 JPH0672247 B2 JP H0672247B2 JP 15017388 A JP15017388 A JP 15017388A JP 15017388 A JP15017388 A JP 15017388A JP H0672247 B2 JPH0672247 B2 JP H0672247B2
- Authority
- JP
- Japan
- Prior art keywords
- powder
- metal
- ultrafine
- metal powder
- vapor
- 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.)
- Expired - Lifetime
Links
- 239000000843 powder Substances 0.000 title claims description 41
- 229910052751 metal Inorganic materials 0.000 title claims description 30
- 239000002184 metal Substances 0.000 title claims description 30
- 238000000034 method Methods 0.000 title claims description 19
- 238000007670 refining Methods 0.000 title description 2
- 239000012808 vapor phase Substances 0.000 claims description 14
- 239000012298 atmosphere Substances 0.000 claims description 13
- 238000004140 cleaning Methods 0.000 claims description 13
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 11
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 11
- 150000004820 halides Chemical class 0.000 claims description 11
- 229910001507 metal halide Inorganic materials 0.000 claims description 11
- 150000005309 metal halides Chemical class 0.000 claims description 11
- 230000001590 oxidative effect Effects 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 11
- 238000000746 purification Methods 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 12
- 239000007789 gas Substances 0.000 description 9
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 8
- 229910052801 chlorine Inorganic materials 0.000 description 8
- 239000000460 chlorine Substances 0.000 description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 4
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 230000003247 decreasing effect Effects 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000010828 elution Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 150000004767 nitrides Chemical class 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- 229910001111 Fine metal Inorganic materials 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- 229910001337 iron nitride Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000010944 silver (metal) Substances 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Landscapes
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Description
【発明の詳細な説明】 〈産業上の利用分野〉 本発明は金属ハロゲン化物の蒸気を気相還元することに
より得られた金属超微粉あるいは金属微粉中に含有され
る不純物としてのハロゲンの除去に関するものである。DETAILED DESCRIPTION OF THE INVENTION <Field of Industrial Application> The present invention relates to removal of halogen as an impurity contained in ultrafine metal powder or fine metal powder obtained by vapor phase reduction of vapor of metal halide. It is a thing.
〈従来技術〉 金属ハロゲン化物の気相還元において得られた金属超微
粉中に残留するハロゲン化物は金属超微粉の耐錆性を阻
害するほか、例えば金属超微粉を導電ペーストに使用す
る場合マイグレーションを引き起こす等の問題があり、
その除去が必要である。<Prior Art> The halide remaining in the ultrafine metal powder obtained in the vapor phase reduction of the metal halide impairs the rust resistance of the ultrafine metal powder and, for example, migration occurs when the ultrafine metal powder is used in a conductive paste. There are problems such as causing
Its removal is necessary.
従来、特開昭60-67603号公報に金属ハロゲン化物の気相
還元法で得られた金属超微粉を水洗して付着ハロゲン化
物を取り除き、その後乾燥時に自然発火を防ぐために制
御された酸素を含むガスにより徐酸化する方法が開示さ
れている。この方法の実施例には、鉄−30％コバルト粉
に処理を施し、塩素濃度が2.43％から30ppmに低下した
と報告されているが、10分／回の撹拌，洗浄を10回繰り
返しており、長時間を要している。また、この方法は、
水に溶解しないハロゲン化物に対しては適用が不可能で
ある。Conventionally, JP-A-60-67603 discloses that ultrafine metal powder obtained by a vapor phase reduction method of metal halides is washed with water to remove adhered halides, and then contains oxygen controlled to prevent spontaneous ignition during drying. A method of gradually oxidizing by gas is disclosed. In the example of this method, it was reported that iron-30% cobalt powder was treated, and the chlorine concentration was lowered from 2.43% to 30 ppm, but 10 minutes / time stirring and washing were repeated 10 times. , Takes a long time. Also, this method
It is not applicable to halides that do not dissolve in water.
また特開昭60-174807号公報においても金属ハロゲン化
物の気相還元で得られた金属および金属窒化物の超微粉
を水洗し、未反応ハロゲン化物および副生成物を除去す
る方法が開示されている。実施例には、塩化鉄のアンモ
ニアによる還元で得られた窒化鉄，金属鉄の水による撹
拌，洗浄が示されているが、１時間／回の撹拌，洗浄を
３回繰り返しており、長時間を要している。しかも、Ｘ
線のピークが消滅していると報告されているだけで、濃
度値は述べられていないが、0.1％以下程度と推測され
る。Further, JP-A-60-174807 also discloses a method of washing unreacted halide and by-products by washing ultrafine powder of metal and metal nitride obtained by vapor phase reduction of metal halide with water. There is. In the examples, stirring and washing of iron nitride and metallic iron obtained by reduction of iron chloride with ammonia are carried out with water, but stirring and washing with 1 hour / time are repeated 3 times for a long time. Is needed. Moreover, X
Although it is reported that the line peak disappears, the concentration value is not stated, but it is estimated to be about 0.1% or less.
また特開昭61-48506号公報には、金属ハロゲン化物の気
相還元により得られた金属、および金属窒化物微粒子中
のハロゲン化物及び副生成物を溶解する酸を用いて洗浄
する方法が開示されている。しかし、この方法でも不純
物の除去はＸ線のピークが消滅する程度であり、また薄
い酸では長時間を要し、濃い酸では金属，金属窒化物粉
自体が溶解してしまう。Further, Japanese Patent Application Laid-Open No. 61-48506 discloses a method of cleaning a metal obtained by vapor phase reduction of a metal halide and an acid that dissolves a halide and by-products in metal nitride fine particles. Has been done. However, even with this method, the removal of impurities is such that the X-ray peak disappears, a long time is required with a thin acid, and a metal or metal nitride powder itself is dissolved with a concentrated acid.
〈発明が解決しようとする課題〉 本発明は、金属ハロゲン化物の蒸気を気相還元すること
により得られた金属超微粉中および微粉中の未反応ハロ
ゲン化物を除去するにあたって、洗浄時間の比較的短
い、また水に不溶なハロゲン化物にも適用でき、かつ本
洗浄による金属粉自体の酸化に起因する溶解損失の殆ん
どない効率的な金属超微粉の精製方法を提案するもので
ある。<Problems to be Solved by the Invention> The present invention, in removing the unreacted halide in the ultrafine metal powder and fine powder obtained by vapor-phase reduction of the vapor of the metal halide, a relatively long cleaning time The present invention proposes an efficient method for refining ultrafine metal powders which is short and can be applied to water-insoluble halides, and causes almost no dissolution loss due to oxidation of the metal powders by the main cleaning.
〈課題解決のための手段〉 本発明の第１は、金属ハロゲン化物の蒸気を気相還元す
ることにより得られた金属超微粉中の残留ハロゲン化物
の除去にあたって、該金属超微粉をアンモニア水を用い
て洗浄することを特徴とする金属超微粉の精製方法であ
る。<Means for Solving the Problem> The first aspect of the present invention is to remove residual metal halide in metal ultrafine powder obtained by vapor-phase reduction of vapor of metal halide, and to remove the metal ultrafine powder from aqueous ammonia. It is a method for purifying ultrafine metal powder, which is characterized in that it is used for washing.
本発明の第２は、上記洗浄を非酸化性雰囲気中で行うこ
とを特徴とする金属超微粉の精製方法である。The second aspect of the present invention is a method for purifying ultrafine metal powder, characterized in that the above-mentioned cleaning is performed in a non-oxidizing atmosphere.
〈作用〉 第１図に本発明を具体化したフローチャートを示す。<Operation> FIG. 1 shows a flowchart embodying the present invention.
まず、洗浄液には望しくは溶存酸素を十分除去したアン
モニア水を用いる。アンモニア濃度は特に規定しない
が、１〜10wt％が好ましい。次に非酸化性雰囲気中で、
洗浄液を未処理粉に入れた後、１〜20分の撹拌，洗浄を
行う。ここでの非酸化性雰囲気としてはAr,He,N2等の不
活性ガス、H2，CH4等の還元ガス、燃焼排ガス等の非酸
化性ガス雰囲気あるいは真空雰囲気が利用できる。本処
理を非酸化性雰囲気中で行うことにより、本精製法が適
用できる金属超微粉において、Cu,Fe,Ni等の洗浄時の溶
解損失を低減できる。ただし、Ag,Au,Pt,Pd等の貴金属
については、必ずしも非酸化性雰囲気中でなくとも溶解
損失を伴うことなく本発明の目的である残留ハロゲン化
物の除去を達成できる。洗浄方法としては、超音波また
は機械的撹拌を用い、洗浄回数は１〜３回で十分であ
る。３回を超えて洗浄してもかまわないが、経済性と残
留ハロゲン量の関係からその必要は殆んどない。First, as a cleaning solution, ammonia water from which dissolved oxygen is sufficiently removed is preferably used. Ammonia concentration is not particularly specified, but 1 to 10 wt% is preferable. Then in a non-oxidizing atmosphere,
After putting the cleaning liquid in the untreated powder, stir and wash for 1 to 20 minutes. As the non-oxidizing atmosphere here, an inert gas such as Ar, He or N 2 , a reducing gas such as H 2 or CH 4 , a non-oxidizing gas atmosphere such as combustion exhaust gas or a vacuum atmosphere can be used. By performing this treatment in a non-oxidizing atmosphere, it is possible to reduce dissolution loss of Cu, Fe, Ni, etc. during cleaning in the ultrafine metal powder to which the present purification method can be applied. However, for noble metals such as Ag, Au, Pt, and Pd, the removal of residual halide, which is the object of the present invention, can be achieved without being accompanied by dissolution loss even in a non-oxidizing atmosphere. As a cleaning method, ultrasonic waves or mechanical agitation is used, and the number of times of cleaning is 1 to 3 times. It may be washed more than three times, but it is hardly necessary in view of the economical efficiency and the amount of residual halogen.
その後、精製粉とアンモニア洗浄液の分離を非酸化性ガ
ス中で吸引ろ過等により行う。ろ過された精製粉は、非
酸化性雰囲気中で乾燥し、非酸化性ガス、または真空中
に保存する。Then, the purified powder and the ammonia cleaning liquid are separated by suction filtration or the like in a non-oxidizing gas. The filtered purified powder is dried in a non-oxidizing atmosphere and stored in a non-oxidizing gas or vacuum.
この精製方法に適用できる金属超微粉，微粉は、金属ハ
ロゲン化物の気相還元により得られるAu,Ag,Cu,Ni,Co,F
e,Mn,Cd,Cr,Ti,Pt,Pd,Ge,Al,Ga,Bi等で、アンモニア水
中で、そのハロゲン化物がアンモニア錯体を形成するも
のである。The ultrafine metal powders and fine powders applicable to this purification method are Au, Ag, Cu, Ni, Co and F obtained by vapor phase reduction of metal halides.
e, Mn, Cd, Cr, Ti, Pt, Pd, Ge, Al, Ga, Bi, etc., whose halide forms an ammonia complex in aqueous ammonia.
なお、一般にその粒度により金属超微粉と微粉を区別し
ているが、本発明の金属超微粉には一般の金属微粉も当
然その範囲に含むものである。It should be noted that, although metal ultrafine powder and fine powder are generally distinguished by the particle size thereof, the metal ultrafine powder of the present invention naturally includes general metal fine powder.
〈実施例〉 実施例−１ 第１図のフローに従って、塩化銅の気相水素還元により
得られた銅超微粉（平均粒径0.3μｍ）の精製を実施し
た。Arガス雰囲気中で、未精製粉5gに対し溶存酸素を除
去した５％アンモニア水100ccを混合し、超音波洗浄に
より20分間の撹拌を行った。この撹拌を２回繰り返した
後、吸引ろ過，真空中乾燥をすることにより、塩素含有
量は3.25％から10ppm以下まで低下した。しかも銅粉自
体のアンモニア水への溶解は認められなかった。<Example> Example-1 According to the flow of Fig. 1, ultrafine copper powder (average particle size 0.3 µm) obtained by vapor-phase hydrogen reduction of copper chloride was purified. In an Ar gas atmosphere, 5 g of unpurified powder was mixed with 100 cc of 5% ammonia water from which dissolved oxygen was removed, and the mixture was stirred for 20 minutes by ultrasonic cleaning. After repeating this stirring twice, suction filtration and drying in vacuum reduced the chlorine content from 3.25% to 10 ppm or less. Moreover, no dissolution of the copper powder itself in ammonia water was observed.
実施例−２ 実施例−１で用いたものと同じ銅超微粉の精製におい
て、N2ガス雰囲気中で、未精製粉10gに対して、溶存酸
素を除去した2.5％アンモニア水150ccで超音波による撹
拌，洗浄を10分／回で３回の処理をした。塩素含有量は
3.25％から10ppm以下に低下し、銅粉自体の溶出は認め
られなかった。In the same copper ultrafine purification as used in Example -2 Example -1, with N 2 gas atmosphere for crude powder 10 g, by ultrasound with 2.5% aqueous ammonia 150cc removing the dissolved oxygen Stirring and washing were carried out 3 times at 10 minutes / time. The chlorine content is
It decreased from 3.25% to 10ppm or less, and no elution of copper powder itself was observed.
実施例−３ 塩化銀の水素還元により得られた銀超微粉（平均粒径0.
5μｍ）の精製において、N2ガス雰囲気中で、未精製粉5
gに対し溶存酸素を除去した５％アンモニア水100ccで超
音波による撹拌，洗浄を20分／回で２回行った。塩素含
有量は5.2％から10ppm以下に低下し、銀粉自体の溶出は
認められなかった。Example 3 Ultrafine silver powder obtained by hydrogen reduction of silver chloride (average particle size: 0.
5 μm) in the N 2 gas atmosphere, unrefined powder 5
For 5 g, 100 cc of 5% ammonia water from which dissolved oxygen was removed was ultrasonically stirred and washed twice for 20 minutes / time. The chlorine content decreased from 5.2% to 10 ppm or less, and no elution of silver powder itself was observed.
実施例−４ 塩化ニッケルの水素還元により得られたNi超微粉（平均
粒径0.08μｍ）の精製において、N2雰囲気中で未精製粉
5gに対し溶存酸素を除去した５％アンモニア水100ccで
超音波による撹拌，洗浄を20分／回で２回処理した。塩
素含有量は3.3％から10ppm以下に低下し、Ni粉自体の溶
出は認められなかった。Example 4 In the purification of Ni ultrafine powder (average particle size 0.08 μm) obtained by hydrogen reduction of nickel chloride, an unpurified powder in N 2 atmosphere
For 5 g, 100 cc of 5% ammonia water from which dissolved oxygen was removed was subjected to ultrasonic agitation and washing twice at 20 minutes / time. The chlorine content decreased from 3.3% to 10 ppm or less, and no elution of the Ni powder itself was observed.
比較例−１ 塩化銅の気相還元により製造した銅超微粉を水で洗浄し
た。未精製粉1gに対し水100ccを入れ、超音波洗浄によ
る30分／回×５回の撹拌，洗浄で、塩素含有量は3.0％
から１％にしか低下しなかった。Comparative Example-1 Ultrafine copper powder produced by vapor-phase reduction of copper chloride was washed with water. 100g of water was added to 1g of unrefined powder, and the chlorine content was 3.0% after 30 minutes of ultrasonic cleaning and 5 times of stirring and cleaning.
Fell to only 1%.
比較例−２ 塩化銅の気相還元により製造した銅超微粉を塩酸で洗浄
を行った。未精製粉2.5gに対し、２規定の塩酸150ccを
加えて40分間超音波洗浄を行った後440mlの純水で洗浄
し、ろ過，乾燥を行った。この方法では塩素含有量は4.
6％から0.5％までしか低下しなかった。Comparative Example-2 Ultrafine copper powder produced by vapor-phase reduction of copper chloride was washed with hydrochloric acid. To 2.5 g of unrefined powder, 150 cc of 2N hydrochloric acid was added, ultrasonically washed for 40 minutes, then washed with 440 ml of pure water, filtered and dried. With this method, the chlorine content is 4.
It fell only from 6% to 0.5%.
比較例−３ 塩化銅の気相還元により得られた銅超微粉を大気中で５
％アンモニア水で洗浄を行った。未精製粉5gに対し５％
アンモニア水100ccを加え超音波で20分／回で３回の洗
浄後、ろ過，乾燥した結果、塩素含有量は2.8％から50p
pm以下に低下したものの酸化が著しく進行しており、酸
素含有量が0.2％から８％に増加した。また銅粉自体も2
0％程度溶出した。Comparative Example-3 An ultrafine copper powder obtained by vapor-phase reduction of copper chloride was used in the atmosphere 5
Washing was performed with aqueous ammonia. 5% for 5 g unrefined flour
After adding 100 cc of ammonia water and ultrasonically washing for 3 times at 20 minutes / time, filtering and drying, the chlorine content is 2.8% to 50p
Although it was reduced to pm or less, the oxidation was significantly advanced, and the oxygen content was increased from 0.2% to 8%. Also the copper powder itself is 2
About 0% was eluted.
〈発明の効果〉 本発明の精製法により、金属ハロゲン化物の気相還元に
より製造した金属超微粉や微粉中の未反応ハロゲン化物
が、従来法に対し極低濃度まで、かつ短時間で、かつ金
属の酸化，溶出を伴うことなく除去できるようになっ
た。<Effects of the Invention> By the purification method of the present invention, the unreacted halide in the ultrafine metal powder or fine powder produced by the vapor phase reduction of the metal halide is extremely low concentration compared to the conventional method, and in a short time, and It is now possible to remove metal without being oxidized or eluted.
第１図は、本発明になる洗浄工程を示す図である。 FIG. 1 is a diagram showing a cleaning process according to the present invention.
Claims (2)
とにより得られた金属超微粉中の残留ハロゲン化物の除
去にあたって、該金属超微粉をアンモニア水を用いて洗
浄することを特徴とする金属超微粉の精製方法。1. A metal which is characterized by washing the ultrafine metal powder with ammonia water when removing the residual halide in the ultrafine metal powder obtained by vapor-phase reduction of the vapor of the metal halide. Ultrafine powder purification method.
行うことを特徴とする金属超微粉の精製方法。2. A method for purifying ultrafine metal powder, wherein the cleaning according to claim 1 is performed in a non-oxidizing atmosphere.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15017388A JPH0672247B2 (en) | 1988-06-20 | 1988-06-20 | Method for refining ultrafine metal powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15017388A JPH0672247B2 (en) | 1988-06-20 | 1988-06-20 | Method for refining ultrafine metal powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01319610A JPH01319610A (en) | 1989-12-25 |
| JPH0672247B2 true JPH0672247B2 (en) | 1994-09-14 |
Family
ID=15491098
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP15017388A Expired - Lifetime JPH0672247B2 (en) | 1988-06-20 | 1988-06-20 | Method for refining ultrafine metal powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0672247B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SG10201402033SA (en) * | 2009-05-05 | 2014-08-28 | Cambrios Technologies Corp | Reliable and durable conductive films comprising metal nanostructures |
| JP2014001455A (en) * | 2013-06-28 | 2014-01-09 | Sumitomo Metal Mining Co Ltd | Silver powder |
-
1988
- 1988-06-20 JP JP15017388A patent/JPH0672247B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01319610A (en) | 1989-12-25 |
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