JPS63270404A - Production of indium metal fine powder - Google Patents
Production of indium metal fine powderInfo
- Publication number
- JPS63270404A JPS63270404A JP10144387A JP10144387A JPS63270404A JP S63270404 A JPS63270404 A JP S63270404A JP 10144387 A JP10144387 A JP 10144387A JP 10144387 A JP10144387 A JP 10144387A JP S63270404 A JPS63270404 A JP S63270404A
- Authority
- JP
- Japan
- Prior art keywords
- indium
- fine powder
- metal fine
- indium metal
- methanol
- 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.)
- Pending
Links
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 30
- 239000002184 metal Substances 0.000 title claims abstract description 30
- 229910052738 indium Inorganic materials 0.000 title claims abstract description 27
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 239000000843 powder Substances 0.000 title claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 9
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 9
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims abstract description 9
- 150000002471 indium Chemical class 0.000 claims abstract description 4
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 claims abstract description 4
- 239000002904 solvent Substances 0.000 claims abstract description 4
- XURCIPRUUASYLR-UHFFFAOYSA-N Omeprazole sulfide Chemical compound N=1C2=CC(OC)=CC=C2NC=1SCC1=NC=C(C)C(OC)=C1C XURCIPRUUASYLR-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910000337 indium(III) sulfate Inorganic materials 0.000 claims abstract 2
- XGCKLPDYTQRDTR-UHFFFAOYSA-H indium(iii) sulfate Chemical compound [In+3].[In+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O XGCKLPDYTQRDTR-UHFFFAOYSA-H 0.000 claims abstract 2
- MOOAHMCRPCTRLV-UHFFFAOYSA-N boron sodium Chemical compound [B].[Na] MOOAHMCRPCTRLV-UHFFFAOYSA-N 0.000 claims description 3
- 239000012279 sodium borohydride Substances 0.000 abstract description 7
- 229910000033 sodium borohydride Inorganic materials 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 5
- 238000010908 decantation Methods 0.000 abstract description 4
- 150000003839 salts Chemical class 0.000 abstract description 3
- 238000004506 ultrasonic cleaning Methods 0.000 abstract description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 230000003111 delayed effect Effects 0.000 description 2
- GPYPVKIFOKLUGD-UHFFFAOYSA-N gold indium Chemical compound [In].[Au] GPYPVKIFOKLUGD-UHFFFAOYSA-N 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、コンデンサー、トランジスターなどの電子部
品の内部電極又はソルダーなどに利用されているインジ
ウム金属微粉の製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for producing fine indium metal powder used for internal electrodes or solders of electronic components such as capacitors and transistors.
従来、インジウム金属微粉を製造する方法としては、イ
ンジウム金属蒸気を急冷する方法やインジウム金属塩を
水に溶解して亜鉛粉末又は水素化硼素ナトリウム等の還
元剤で還元する方法がある。Conventionally, methods for producing fine indium metal powder include a method of rapidly cooling indium metal vapor and a method of dissolving an indium metal salt in water and reducing it with a reducing agent such as zinc powder or sodium borohydride.
上記従来のインジウム金属蒸気を急冷する方法はインジ
ウム金属の融点が一般の金属と比較して１５６．６℃と
低いので、急冷によって生成されたインジウム金属微粉
は相互に融着し易く微小径の微粉を製造し難い欠点があ
る。又、上記従来のインジウム金属塩の水溶液を還元す
る方法は、生成して来るインジウム金属が凝集してスポ
ンジ状になり易く微粉とはなり難い欠点を有する。上記
従来の方法では５０ｐｍ以下のインジウム金属粉を得る
ことが困難であり、これらの欠点のため微小径のインジ
ウム金属微粉の商品化が遅れ、鉄粉や銅粉の様に工業的
規模で供給する事が大幅に遅れていた。In the conventional method of rapidly cooling indium metal vapor, the melting point of indium metal is 156.6°C, which is lower than that of ordinary metals, so the indium metal fine powder generated by rapid cooling easily fuses with each other, resulting in fine diameter particles. There are drawbacks that make it difficult to manufacture. Furthermore, the conventional method of reducing an aqueous solution of an indium metal salt has the disadvantage that the generated indium metal tends to aggregate and become spongy, and is difficult to turn into fine powder. It is difficult to obtain indium metal powder with a particle diameter of 50 pm or less using the above conventional methods, and these drawbacks have delayed the commercialization of micro-diameter indium metal fine powder, which has not been supplied on an industrial scale like iron powder or copper powder. Things were delayed a lot.
本発明は、上記の問題点を解決し、紛擾１乃至１０μｍ
のインジウム金属微粉を安定して大量に供給する方法を
提供することを目的とする。The present invention solves the above-mentioned problems,
The purpose of the present invention is to provide a method for stably supplying a large amount of indium metal fine powder.
本発明は、メタノール、エタノール、１−プロパノール
、２−プロパノール、１−ブタノール、２−ブタノール
からなる群の中より選ばれた１種類以上を成分とする溶
剤に対し、塩化インジウム、硝酸インジウム、硫酸イン
ジウムからなる群の中より選ばれたインジウム塩を溶解
し、これを水素化硼素ナトリウムで還元して、インジウ
ム金属微粉を生成させることを特徴とするインジウム金
属微粉の製造方法である。The present invention provides indium chloride, indium nitrate, and sulfuric acid for a solvent containing one or more selected from the group consisting of methanol, ethanol, 1-propanol, 2-propanol, 1-butanol, and 2-butanol. This is a method for producing indium metal fine powder, which is characterized by dissolving an indium salt selected from the group consisting of indium and reducing it with sodium boron hydride to produce indium metal fine powder.
インジウム塩の溶解している溶液を水素化硼素ナトリウ
ムで還元する場合、溶液に水素化硼素ナトリウムを添加
して行う。水素化硼素ナトリウムによる還元は反応熱を
伴うので急速な添加は溶液の温度を急上昇させて沸騰現
象を生じさせ易くなり、生成するインジウム金属はゲル
状の塊状になる場合がある。水素化硼素ナトリウムの添
加速度を調整したり、溶液を洗浄したりするなどの方法
によって沸騰現象を回避することが望ましい。インジウ
ム金属微粉を冷却する場合は濾過方式は金属微粉によっ
て濾紙の目詰まりを生じ易く好ましくないので、デカン
テーションによる洗浄を行う。When reducing a solution in which an indium salt is dissolved with sodium borohydride, sodium borohydride is added to the solution. Since reduction with sodium borohydride is accompanied by heat of reaction, rapid addition tends to rapidly raise the temperature of the solution and cause a boiling phenomenon, and the resulting indium metal may form a gel-like mass. It is desirable to avoid the boiling phenomenon by adjusting the addition rate of sodium borohydride, washing the solution, etc. When cooling indium metal fine powder, filtration is not preferable because the metal fine powder tends to clog the filter paper, so cleaning is performed by decantation.
この場合、水による洗浄はインジウム金属が酸化され易
いのでメタノールを用いる。デカンテーションによる洗
浄ではインジウム金属微粉に付着している塩化ナトリウ
ムが完全に除却しきれない場合があるので、超音波洗浄
器を用いてメタノール中でインジウム金属微粉を分散さ
せながら洗浄することが好ましい。このようにして入手
されたインジウム金属微粉はＸ線回折により不純物とし
ての塩化ナトリウムは完全に除却されていることが確認
された０本発明によりえられたインジウム金属微粉の粒
径はｌ乃至１０μｍであることが電子顕微鏡により確認
された。In this case, since indium metal is easily oxidized when cleaning with water, methanol is used. Since the sodium chloride adhering to the indium metal fine powder may not be completely removed by cleaning by decantation, it is preferable to wash the indium metal fine powder while dispersing it in methanol using an ultrasonic cleaner. It was confirmed by X-ray diffraction that sodium chloride as an impurity was completely removed from the indium metal fine powder obtained in this way. This was confirmed using an electron microscope.
無水塩化インジウム５００ｇをメタノール５０００ ｍ
ｌに溶解し、水素化硼素ナトリウム２５０ｇを１回の滴
下量１０ｇとして１０分間滴下してインジウム金ｒ％微
粉２２５ｇを得た。このインジウム金ｙＸ微粉に対しメ
タノールによるデカンテーション操作を３回繰返し、そ
の後超音波洗浄を３回行い、粒径１乃至１０μｍのイン
ジウム金属微粉を総量２２５ｇ得た。収率は９０％であ
った。500 g of anhydrous indium chloride and 5000 m of methanol
250 g of sodium boron hydride was added dropwise for 10 minutes to obtain 225 g of indium gold r% fine powder. The decantation operation with methanol was repeated three times for this indium gold yX fine powder, and then the ultrasonic cleaning was performed three times to obtain a total of 225 g of indium metal fine powder with a particle size of 1 to 10 μm. The yield was 90%.
本発明により電子部品業界から望まれていた粒径１乃至
１０μｍのインジウム金属微粉を工業的規模で容易に製
造することが可能になった。The present invention has made it possible to easily produce on an industrial scale indium metal fine powder with a particle size of 1 to 10 μm, which has been desired by the electronic parts industry.
Claims (1)
パノール、１−ブタノール、２−ブタノールからなる群
の中より選ばれた１種類以上を成分とする溶剤に対し、
塩化インジウム、硝酸インジウム、硫酸インジウムから
なる群の中より選ばれたインジウム塩を溶解し、これを
水素化硼素ナトリウムで還元してインジウム金属微粉を
生成させることを特徴とするインジウム金属微粉の製造
方法。For a solvent containing one or more types selected from the group consisting of methanol, ethanol, 1-propanol, 2-propanol, 1-butanol, and 2-butanol,
A method for producing indium metal fine powder, which comprises dissolving an indium salt selected from the group consisting of indium chloride, indium nitrate, and indium sulfate, and reducing this with sodium boron hydride to produce indium metal fine powder. .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10144387A JPS63270404A (en) | 1987-04-24 | 1987-04-24 | Production of indium metal fine powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10144387A JPS63270404A (en) | 1987-04-24 | 1987-04-24 | Production of indium metal fine powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63270404A true JPS63270404A (en) | 1988-11-08 |
Family
ID=14300831
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10144387A Pending JPS63270404A (en) | 1987-04-24 | 1987-04-24 | Production of indium metal fine powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63270404A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7166143B2 (en) * | 2002-04-05 | 2007-01-23 | Otkrytoe Aktsionernoe Obschestvo “Chelyabinsky Tsinkovy Zavod” | Method for producing indium powder |
| WO2007055422A1 (en) * | 2005-11-10 | 2007-05-18 | Sumitomo Metal Mining Co., Ltd. | Indium nanowire, oxide nanowire, electroconductive oxide nanowire, and production process thereof |
| CN101879604A (en) * | 2010-06-02 | 2010-11-10 | 浙江大学 | Preparation method and application of metallic indium nanometer particle ink |
| CN103990810A (en) * | 2014-05-30 | 2014-08-20 | 洛阳理工学院 | Technology for preparing nanometer indium powder |
-
1987
- 1987-04-24 JP JP10144387A patent/JPS63270404A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7166143B2 (en) * | 2002-04-05 | 2007-01-23 | Otkrytoe Aktsionernoe Obschestvo “Chelyabinsky Tsinkovy Zavod” | Method for producing indium powder |
| WO2007055422A1 (en) * | 2005-11-10 | 2007-05-18 | Sumitomo Metal Mining Co., Ltd. | Indium nanowire, oxide nanowire, electroconductive oxide nanowire, and production process thereof |
| US8043409B2 (en) | 2005-11-10 | 2011-10-25 | Sumitomo Metal Mining Co., Ltd. | Indium-based nanowire product, oxide nanowire product, and electroconductive oxide nanowire product, as well as production methods thereof |
| CN101879604A (en) * | 2010-06-02 | 2010-11-10 | 浙江大学 | Preparation method and application of metallic indium nanometer particle ink |
| CN103990810A (en) * | 2014-05-30 | 2014-08-20 | 洛阳理工学院 | Technology for preparing nanometer indium powder |
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