JP2903106B2 - Ultra-fine gold-copper alloy particles having a regular icosahedral structure and method for producing the same - Google Patents
Ultra-fine gold-copper alloy particles having a regular icosahedral structure and method for producing the sameInfo
- Publication number
- JP2903106B2 JP2903106B2 JP9054516A JP5451697A JP2903106B2 JP 2903106 B2 JP2903106 B2 JP 2903106B2 JP 9054516 A JP9054516 A JP 9054516A JP 5451697 A JP5451697 A JP 5451697A JP 2903106 B2 JP2903106 B2 JP 2903106B2
- Authority
- JP
- Japan
- Prior art keywords
- copper alloy
- particles
- gold
- ultrafine
- alloy particles
- 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
- 239000002245 particle Substances 0.000 title claims description 42
- 229910000881 Cu alloy Inorganic materials 0.000 title claims description 31
- QRJOYPHTNNOAOJ-UHFFFAOYSA-N copper gold Chemical compound [Cu].[Au] QRJOYPHTNNOAOJ-UHFFFAOYSA-N 0.000 title claims description 31
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 27
- 239000011882 ultra-fine particle Substances 0.000 claims description 22
- 239000000956 alloy Substances 0.000 claims description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 8
- 229910052802 copper Inorganic materials 0.000 claims description 8
- 239000010949 copper Substances 0.000 claims description 8
- 238000001704 evaporation Methods 0.000 claims description 8
- 239000007789 gas Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 229910003481 amorphous carbon Inorganic materials 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 229910001316 Ag alloy Inorganic materials 0.000 description 1
- 229910001020 Au alloy Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
Landscapes
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
- Physical Vapour Deposition (AREA)
Description
【０００１】[0001]
【発明の属する技術分野】本発明は正２０面体構造を有
する金銅合金超微粒子及びその製造方法に関するもので
ある。The present invention relates to ultrafine gold-copper alloy particles having a icosahedral structure and a method for producing the same.
【０００２】[0002]
【従来の技術】ガス中蒸発法を用いることにより、正２
０面体構造（Icosahedral structure:以下「ＩＣ構造」
と略記することもある）を持つ金、銀、パラジウム、コ
バルト等の単元素金属超微粒子が生成することは知られ
ているが、ＩＣ構造を持つ金銅合金超微粒子は知られて
いない。ところで、上記のようにして生成された従来の
超微粒子は、その生成粒子の全てがＩＣ構造を持つもの
ではなく、他の構造（面心立方構造）の粒子が多量混入
している。しかも、それらの超微粒子は、通常構造不安
定で、熱処理を受けると他の構造、特に面心立方構造に
変化する。2. Description of the Related Art By using an in-gas evaporation method, a positive
Icosahedral structure (hereinafter "IC structure")
It is known that ultrafine particles of a single element metal such as gold, silver, palladium, and cobalt are produced, but no ultrafine particles of a gold-copper alloy having an IC structure are known. By the way, in the conventional ultrafine particles generated as described above, not all of the generated particles have an IC structure, and a large amount of particles of another structure (face-centered cubic structure) are mixed. Moreover, these ultrafine particles are usually unstable in structure, and change to another structure, particularly a face-centered cubic structure when subjected to heat treatment.
【０００３】[0003]
【発明が解決しようとする課題】本発明は、正２０面体
構造を持つ構造安定な金属超微粒子及びその製造方法を
提供することをその課題とする。SUMMARY OF THE INVENTION An object of the present invention is to provide structurally stable ultrafine metal particles having a regular icosahedral structure and a method for producing the same.
【０００４】[0004]
【課題を解決するための手段】本発明者らは、前記課題
を解決すべく鋭意研究を重ねた結果、本発明を完成する
に至った。即ち、本発明によれば、１５〜３５モル％の
銅含有量及び６ｎｍ以下の粒径を有し、かつ正２０面体
構造を有することを特徴とする金銅合金超微粒子が提供
される。また、本発明によれば、６〜１５モル％の銅含
有量を有する金銅合金材料をガス中蒸発法を適用して粒
径が６ｎｍ以下の超微粒子を生成させた後、４００〜５
００℃の熱処理を施すことを特徴とする正２０面体構造
を有する金銅合金超微粒子の製造方法が提供される。Means for Solving the Problems The present inventors have made intensive studies to solve the above-mentioned problems, and as a result, have completed the present invention. That is, according to the present invention, there are provided ultrafine gold-copper alloy particles having a copper content of 15 to 35 mol%, a particle size of 6 nm or less, and a icosahedral structure. Further, according to the present invention, a gold-copper alloy material having a copper content of 6 to 15 mol% is applied with an in-gas evaporation method to generate ultrafine particles having a particle size of 6 nm or less, and then 400 to 5 mol%.
A method for producing ultrafine gold-copper alloy particles having a icosahedral structure, characterized by performing a heat treatment at 00 ° C.
【０００５】[0005]
【発明の実施の形態】本発明の金銅合金超微粒子は、粒
径が６ｎｍ以下、好ましくは１〜６ｎｍの範囲のもので
あり、安定したＩＣ構造を有する。この金銅合金超微粒
子は、金銅合金材料にガス中蒸発法を適用して粒径が６
ｎｍ以下の超微粒子を生成させた後、該超微粒子に４０
０〜５００℃の熱処理を施すことにより製造される。本
発明において使用するガス中蒸発法としては、従来の単
元素超微粒子の場合と同様に、抵抗加熱法、プラズマジ
ェット加熱法、誘導加熱法、電子ビーム加熱法、レーザ
ービーム加熱法、アークプラズマ・スパッタリング等の
従来公知の方法を用いることができる。本発明において
使用する金銅合金材料としては、適用されるガス中蒸発
法の種類に応じてインゴット状、棒状等の任意の形状、
形態のものが用いられる。金銅合金材料における銅の含
有量は６〜１５モル％、好ましくは約１０モル％であ
る。BEST MODE FOR CARRYING OUT THE INVENTION The ultrafine gold-copper alloy particles of the present invention have a particle diameter of 6 nm or less, preferably 1 to 6 nm, and have a stable IC structure. The ultrafine gold-copper alloy particles have a particle size of 6 by applying a gas evaporation method to the gold-copper alloy material.
After the generation of ultrafine particles having a size of
It is manufactured by performing a heat treatment at 0 to 500 ° C. The gas evaporation method used in the present invention includes, as in the case of conventional single element ultrafine particles, a resistance heating method, a plasma jet heating method, an induction heating method, an electron beam heating method, a laser beam heating method, an arc plasma heating method, and the like. A conventionally known method such as sputtering can be used. As the gold-copper alloy material used in the present invention, any shape such as ingot shape, rod shape, etc., depending on the type of the applied gas evaporation method,
The form is used. The copper content in the gold-copper alloy material is 6 to 15 mol%, preferably about 10 mol%.
【０００６】本発明により安定なＩＣ構造の金銅合金超
微粒子を製造するには、まず、該金銅合金材料に上記ガ
ス中蒸発法を適用することにより金銅合金の超微粒子を
得る。この場合、ＩＣ構造の安定な粒子を得るには、得
られる金銀合金超微粒子の粒径を６ｎｍ以下にコントロ
ールすることが必要である。この粒径のコントロールは
常法により行うことができ、例えば、金銅合金材料の気
化条件における圧力と、その気化蒸気が冷却微粒子化さ
れる条件における圧力との間の圧力差により調節するこ
とができる。この場合、その圧力差を大きくすることに
より、より小さな粒径の粒子を得ることができる。ま
た、合金中の銅含有量も得られる粒子の粒径に影響を及
ぼし、前記範囲を逸脱すると、６ｎｍ以下の粒径を有す
る粒子を得ることが困難になる。In order to produce ultrafine gold-copper alloy particles having a stable IC structure according to the present invention, first, ultrafine gold-copper alloy particles are obtained by applying the above-mentioned gas evaporation method to the gold-copper alloy material. In this case, in order to obtain particles having a stable IC structure, it is necessary to control the particle size of the obtained ultrafine gold / silver alloy particles to 6 nm or less. The control of the particle size can be performed by a conventional method, for example, it can be adjusted by the pressure difference between the pressure under the vaporization condition of the gold-copper alloy material and the pressure under the condition where the vaporized vapor is cooled and atomized. . In this case, particles having a smaller particle size can be obtained by increasing the pressure difference. Further, the copper content in the alloy also affects the particle size of the obtained particles. If the content is outside the above range, it becomes difficult to obtain particles having a particle size of 6 nm or less.
【０００７】前記のようにして得られる６ｎｍ以下の粒
径を有する金銅合金超微粒子において、そのＩＣ構造を
有するものの割合は約３０％程度であり特定不能な複雑
構造のものが多量混在している。そこで、本発明では、
次に、上記で得た超微粒子に、更に熱処理を施す。この
熱処理により、金銅合金超微粒子の実質的に全てがＩＣ
構造になり、その少なくとも８０％は歪みのない安定し
たＩＣ構造を有する超微粒子に変換される。この熱処理
は、３５０〜５５０℃、好ましくは４００〜５００℃で
３０〜１２０分間、好ましくは４５〜６０分間、真空中
あるいは不活性ガス中で行うことが望ましい。熱処理後
は、金銅合金超微粒子は急冷ではなく、徐冷することが
望ましい。[0007] In the ultrafine gold-copper alloy particles having a particle diameter of 6 nm or less obtained as described above, the ratio of those having an IC structure is about 30%, and a large number of unspecified complicated structures are mixed. . Therefore, in the present invention,
Next, the ultrafine particles obtained above are further subjected to a heat treatment. By this heat treatment, substantially all of the ultra-fine gold-copper alloy particles become IC
Structure, at least 80% of which is converted to ultrafine particles with a stable IC structure without distortion. This heat treatment is desirably performed at 350 to 550 ° C., preferably 400 to 500 ° C., for 30 to 120 minutes, preferably 45 to 60 minutes, in a vacuum or in an inert gas. After the heat treatment, it is desirable that the ultrafine gold-copper alloy particles are not rapidly cooled but gradually cooled.
【０００８】[0008]
【実施例】次に本発明を実施例により詳述する。Next, the present invention will be described in detail with reference to examples.
【０００９】実施例 銅含有量が２５重量％の金銅合金インゴットを作製し、
この材料を、ガス中蒸発法の中の抵抗加熱法を用い、下
記の条件で、気化させ、得られた蒸気をノズルを介して
沈着チャンバーに導き、非晶質炭素薄膜上に沈着担持さ
せた。 カーボン炉温度： １２２５℃ ヘリウムガス流速： １０リットル／分 生成チャンバー内圧力： ２６ｈＰａ 生成チャンバーと沈着チャンバーとの圧力差： ２０ｈ
Ｐａ 炉と炭素薄膜との間の距離：６５０ｍｍ ノズル径： ４ｍｍ ノズル長： ４００ｍｍEXAMPLE A gold-copper alloy ingot having a copper content of 25% by weight was prepared.
This material was vaporized using a resistance heating method in a gas evaporation method under the following conditions, and the obtained vapor was led to a deposition chamber via a nozzle, and deposited and supported on an amorphous carbon thin film. . Carbon furnace temperature: 1225 ° C Helium gas flow rate: 10 L / min Pressure in the production chamber: 26 hPa Pressure difference between the production chamber and the deposition chamber: 20 h
Pa Distance between furnace and carbon thin film: 650 mm Nozzle diameter: 4 mm Nozzle length: 400 mm
【００１０】このようにして非晶質炭素薄膜上に担持さ
れた金銅合金超微粒子の内部構造を、透過型電子顕微鏡
で観察した。その結果、超微粒子のうち、約３割は歪み
を多く含んだＩＣ構造のものであり、残りの約７割は特
定不能な複雑構造のものであった。[0010] The internal structure of the ultrafine gold-copper alloy particles thus supported on the amorphous carbon thin film was observed with a transmission electron microscope. As a result, about 30% of the ultrafine particles had an IC structure containing a large amount of distortion, and the remaining about 70% had an unspecified complicated structure.
【００１１】次に、上記で得た金銅合金超微粒子を非晶
質炭素薄膜上に担持させたまま、真空中で４５０℃で１
時間熱処理を行った後、５時間かけて室温まで徐冷し
た。そそして、熱処理を施した金銅合金超微粒子につい
て、上記と同様に透過型電子顕微鏡で内部構造を観察し
た。その結果、粒径が６ｎｍ以下の超微粒子はすべてＩ
Ｃ構造に変化し、そのうちの約８割は歪みのない完全な
ＩＣ構造であり、外形も良く整っていた。一方、粒径が
６ｎｍより大きい金銅合金超微粒子はすべて通常のバル
クの結晶構造である面心立方構造に変化していた。Next, with the ultrafine gold-copper alloy particles obtained above being carried on an amorphous carbon thin film,
After heat treatment for an hour, the mixture was gradually cooled to room temperature over 5 hours. Then, the internal structure of the heat-treated ultrafine gold-copper alloy particles was observed with a transmission electron microscope in the same manner as described above. As a result, all the ultrafine particles having a particle size of 6 nm or less
The structure changed to a C structure, and about 80% of the structure was a complete IC structure without distortion, and the outer shape was well arranged. On the other hand, all the ultrafine gold-copper alloy particles having a particle size larger than 6 nm changed to a face-centered cubic structure which is a normal bulk crystal structure.
【００１２】比較例１ 金銅合金材料の代わりに金単独材料を用いた以外は実施
例１と同様にして超微粒子を生成させた後、熱処理を施
した。そして熱処理前の超微粒子及び熱処理後の超微粒
子について、実施例１と同様な観察を行った。その結
果、熱処理前の超微粒子は、正１０面体構造のものと、
面心立方構造のものとが混在したものであった。一方、
熱処理後の超微粒子は、すべて面心立方構造に変化して
いた。Comparative Example 1 Ultrafine particles were produced in the same manner as in Example 1 except that a gold-only material was used instead of the gold-copper alloy material, and then heat treatment was performed. The same observations as in Example 1 were performed on the ultrafine particles before and after the heat treatment. As a result, the ultrafine particles before heat treatment have a regular decahedral structure,
It had a mixture of a face-centered cubic structure. on the other hand,
All of the ultrafine particles after the heat treatment changed to a face-centered cubic structure.
【００１３】比較例２ 金銅合金材料の代わりに銅単独材料を用いた以外は実施
例１と同様にして超微粒子を生成させた後、熱処理を施
した。そして熱処理前の超微粒子及び熱処理後の超微粒
子について、実施例１と同様な観察を行った。その結
果、熱処理前の超微粒子は、特定不能な複雑構造のもの
と、面心立方構造のものとが混在したものであった。ま
た、熱処理後の超微粒子も、特定不能な複雑構造のもの
と、面心立方構造のものとが混在したもので、熱処理の
前後であまり変化はなかった。Comparative Example 2 Ultrafine particles were produced in the same manner as in Example 1 except that a copper-only material was used instead of the gold-copper alloy material, and then heat treatment was performed. The same observations as in Example 1 were performed on the ultrafine particles before and after the heat treatment. As a result, the ultrafine particles before the heat treatment were a mixture of an unspecified complex structure and a face-centered cubic structure. The ultrafine particles after the heat treatment also had a mixture of an unspecified complex structure and a face-centered cubic structure, and did not change much before and after the heat treatment.
【００１４】上記実施例及び比較例１、２から次のこと
がわかる。即ち、１種類の原子のみからＩＣ構造の超微
粒子を生成させるのは困難であり、また熱処理によって
も安定したＩＣ構造を得ることは困難である。ところ
が、金銅合金では、粒径が６ｎｍ以下の超微粒子は熱処
理を施すことにより、安定したＩＣ構造とすることがで
きる。The following can be seen from the above embodiment and comparative examples 1 and 2. That is, it is difficult to generate ultrafine particles having an IC structure from only one kind of atoms, and it is also difficult to obtain a stable IC structure by heat treatment. However, in a gold-copper alloy, ultra-fine particles having a particle size of 6 nm or less can be subjected to a heat treatment to have a stable IC structure.
【００１５】[0015]
【発明の効果】本発明の正２０面体構造を有する金銅合
金超微粒子は、構造安定なもので、その取扱いに際して
構造変化することはない。本発明の金銅合金超微粒子
は、粒体状又は成形体状で取扱われるが、高密度な表面
原子配置構造特性を有し、触媒材料や、微小電子素子等
として利用することができる。The ultrafine gold-copper alloy particles having an icosahedral structure according to the present invention are structurally stable and do not change in structure when handled. Although the ultrafine gold-copper alloy particles of the present invention are handled in the form of particles or compacts, they have a high-density surface atom arrangement structure characteristic and can be used as catalyst materials, microelectronic elements, and the like.
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 平６−287745（ＪＰ，Ａ) 特開 平７−11309（ＪＰ，Ａ) 特開 平７−126702（ＪＰ，Ａ) 特開 平９−316504（ＪＰ，Ａ) 特開 平９−111316（ＪＰ，Ａ) (58)調査した分野(Int.Cl.6，ＤＢ名) B22F 1/00 B22F 9/02 B22F 9/12 - 9/14 C22C 5/02 C23C 14/00 ────────────────────────────────────────────────── ─── Continuation of the front page (56) References JP-A-6-287745 (JP, A) JP-A-7-11309 (JP, A) JP-A-7-126702 (JP, A) JP-A-9-99 316504 (JP, A) JP-A-9-111316 (JP, A) (58) Fields investigated (Int. Cl. 6 , DB name) B22F 1/00 B22F 9/02 B22F 9/12-9/14 C22C 5/02 C23C 14/00
Claims (2)
以下の粒径を有し、かつ正２０面体構造を有することを
特徴とする金銅合金超微粒子。1. The copper content of 15 to 35 mol% and 6 nm
Ultra-fine gold-copper alloy particles having the following particle diameter and a regular icosahedral structure.
合金材料をガス中蒸発法を適用して粒径が６ｎｍ以下の
超微粒子を生成させた後、４００〜５００℃の熱処理を
施すことを特徴とする正２０面体構造を有する金銅合金
超微粒子の製造方法。2. A gold-copper alloy material having a copper content of 6 to 15 mol% is applied with a gas evaporation method to generate ultrafine particles having a particle size of 6 nm or less, and then subjected to a heat treatment at 400 to 500 ° C. A method for producing ultrafine gold-copper alloy particles having a regular icosahedral structure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9054516A JP2903106B2 (en) | 1997-03-10 | 1997-03-10 | Ultra-fine gold-copper alloy particles having a regular icosahedral structure and method for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9054516A JP2903106B2 (en) | 1997-03-10 | 1997-03-10 | Ultra-fine gold-copper alloy particles having a regular icosahedral structure and method for producing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH10251703A JPH10251703A (en) | 1998-09-22 |
| JP2903106B2 true JP2903106B2 (en) | 1999-06-07 |
Family
ID=12972823
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9054516A Expired - Lifetime JP2903106B2 (en) | 1997-03-10 | 1997-03-10 | Ultra-fine gold-copper alloy particles having a regular icosahedral structure and method for producing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2903106B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20010099547A (en) * | 2000-04-27 | 2001-11-09 | 허승헌 | A design of a nanometer size metal, nonmetal, and alloy particle generator |
| JP4962364B2 (en) * | 2008-03-14 | 2012-06-27 | 富士電機株式会社 | Method for producing metal nanoparticles and metal nanoparticle fixed body |
-
1997
- 1997-03-10 JP JP9054516A patent/JP2903106B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH10251703A (en) | 1998-09-22 |
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