JP2017509784A - Graphene reinforced copper-based composite contact material and method for producing the same - Google Patents

Graphene reinforced copper-based composite contact material and method for producing the same Download PDF

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JP2017509784A
JP2017509784A JP2016537500A JP2016537500A JP2017509784A JP 2017509784 A JP2017509784 A JP 2017509784A JP 2016537500 A JP2016537500 A JP 2016537500A JP 2016537500 A JP2016537500 A JP 2016537500A JP 2017509784 A JP2017509784 A JP 2017509784A
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graphene
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リーチャン リュー
リーチャン リュー
ウェイ ウェン
ウェイ ウェン
ワンファン リン
ワンファン リン
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H1/00—Contacts
    • H01H1/02—Contacts characterised by the material thereof
    • H01H1/021—Composite material
    • H01H1/025—Composite material having copper as the basic material

Abstract

【解決手段】本発明は、酸化物粉末：０．０１〜１０質量％、炭化物粉末：０．０１〜２質量％、残部：厚さ１０ｎｍ以下のグラフェンで被覆された銅粉末又は銅合金粉末からなる、グラフェン補強銅系複合接点材料及びその製造方法を開示した。この銅系複合接点材料は接触抵抗が低くて安定し、耐アーク消耗性及び耐溶着性に優れている利点を有し、従来の銀系接点材料を代替して低圧遮断器、接触器及び継電器に適用することができる。The present invention provides an oxide powder: 0.01 to 10% by mass, a carbide powder: 0.01 to 2% by mass, and a balance: a copper powder or a copper alloy powder coated with graphene having a thickness of 10 nm or less. A graphene-reinforced copper-based composite contact material and a manufacturing method thereof have been disclosed. This copper-based composite contact material has the advantages of low contact resistance and stability, and excellent arc wear resistance and welding resistance. Can be applied to.

Description

本発明は電気接触材料分野に属し、詳しくは低圧電気機器用接点材料に関し、特にグラフェン補強銅系複合接点材料に関するものである。   The present invention belongs to the field of electrical contact materials, and particularly relates to contact materials for low-voltage electrical equipment, and more particularly to graphene-reinforced copper-based composite contact materials.

接点材料は各種のスイッチ、継電器、接触器などの電気機器の重要な材料であり、電流を投入、遮断及び伝送する役割を果たす。現在国内外で多く使用されている接点材料は銀系材料であるが、そのコストが高い。一部の銅系接点材料は使用されているが、その耐酸化性が低く、電気的寿命が短い。主な原因は銅が接触表面に露出しているので、低温耐酸化性が低下し、アークによる消耗が激しくなっている。   The contact material is an important material for electric devices such as various switches, relays, and contactors, and plays a role of supplying, interrupting, and transmitting current. Currently, contact materials that are widely used in Japan and overseas are silver-based materials, but their cost is high. Some copper-based contact materials are used, but their oxidation resistance is low and their electrical life is short. The main cause is that copper is exposed on the contact surface, so the low-temperature oxidation resistance is reduced and the arc wear is increased.

検索を経て、以下の特許は銅系接点材料に関するものである。   After searching, the following patents relate to copper-based contact materials.

１、ＣＮ１２２４７６８Ａの銅系銀フリーカドミウムフリー低圧電気接点合金材料は、主に、補強材（ダイヤモンドなど）及び添加物（Ｚｎ、Ｓｎなど）を用いることで銅系接点材料の電気的特性の改善を図るものである。   1. CN1224768A copper-based silver-free cadmium-free low-voltage electrical contact alloy material mainly uses reinforcing materials (such as diamond) and additives (Zn, Sn, etc.) to improve the electrical characteristics of copper-based contact materials. It is intended.

２、ＣＮ１７６７１０５Ａの低圧電気機器用環境保全型銅系接点材料及び接点の製造方法は、主に、補強材（希土類酸化物）及び添加物（希土類金属元素）を用いることで銅系接点材料の電気的特性の改善を図るものである。   2, CN1767105A environmental protection type copper-based contact material for low-voltage electrical equipment and the manufacturing method of the contact, mainly using a reinforcing material (rare earth oxide) and an additive (rare earth metal element), It is intended to improve the mechanical characteristics.

３、ＣＮ１０１３３５１０２Ａの電気接触要素用の銅系材料は、主に、銅基材に第５、６族元素及び希土類元素を添加する方法で電気的特性の改善を図るものである。   3. The copper-based material for electrical contact elements of CN101335102A is intended to improve electrical characteristics mainly by adding Group 5 and 6 elements and rare earth elements to a copper base material.

４、ＣＮ１０２３２４３３５Ａの複合電気接点材料の製造方法は、カーボンナノチューブ被覆銅を特徴とする銅系接点材料を開示した。   4. CN102324335A composite electrical contact material manufacturing method disclosed a copper-based contact material featuring carbon nanotube-coated copper.

５、ＣＮ１０２２１８５４０Ａのグラフェンと金属とのナノ複合粉末及びその製造方法である。   5, CN102218540A graphene and metal nanocomposite powder and its manufacturing method.

以上の発明のうち、前の３つの特許はいずれも補強材及び添加物を用いる方法で銅系接点材料の改善を図っているが、銅基材に対しては改善を行っていないので、これらの材料の使用に際し、銅が空気やアークにさらされて酸化しやすくなり、接触抵抗に影響を及ぼす。特許４はカーボンナノチューブ被覆銅の接点材料を提案しているが、この材料は製造方法が複雑であり、原料として銅片を使用することにより銅粒子が粗大化してしまい（カーボンナノチューブが完全保護の役割を果たすことができない）、材料内部に一部の銀が含有されて銀フリー化が実現できないなどの問題が存在し、工業的使用が困難である。特許５はグラフェンと金属粉末とを複合化した材料を提案しているが、グラフェンマイクロシートが使用され、金属粒子表面をグラフェンで被覆することができず、金属粒子の完全保護を実現することができない。   Of the above inventions, the previous three patents all attempt to improve the copper-based contact material by a method using a reinforcing material and an additive, but these are not improved for the copper base material. When using these materials, copper is easily oxidized by exposure to air or arc, which affects contact resistance. Patent 4 proposes a carbon nanotube-covered copper contact material, but this material has a complicated manufacturing method, and copper particles are coarsened by using copper pieces as a raw material (carbon nanotubes are completely protected). However, there is a problem that a part of silver is contained in the material and silver free cannot be realized, and industrial use is difficult. Patent 5 proposes a material in which graphene and metal powder are combined, but graphene microsheets are used, and the metal particle surface cannot be coated with graphene, so that complete protection of the metal particles can be realized. Can not.

同様に、従来の粉末混合方法でグラフェン及びカーボンナノチューブを添加して製造した、グラフェン及びカーボンナノチューブを有する銅系接点材料に比べて、これらの方法で製造された材料は、各々の補強材と基材との間にグラフェン又はカーボンナノチューブが分散されていることを確保できないので、品質や性能の不安定性の問題が存在する。   Similarly, compared to copper-based contact materials having graphene and carbon nanotubes, which are produced by adding graphene and carbon nanotubes by a conventional powder mixing method, the materials produced by these methods have different reinforcing materials and substrates. Since it is not possible to ensure that graphene or carbon nanotubes are dispersed between the materials, there are problems of instability of quality and performance.

本発明の第１の目的は、従来技術に存在する欠陥や不足を克服するために、銅系接点材料の耐酸化性が低く、アーク消耗が大きいという問題点を解決することができるとともに、補強材と基材との間に均質に分散しているグラフェン補強銅系複合接点材料を提供することにある。   The first object of the present invention is to solve the problem that the oxidation resistance of the copper-based contact material is low and the arc consumption is large in order to overcome the deficiencies and deficiencies existing in the prior art, and the reinforcement It is to provide a graphene-reinforced copper-based composite contact material that is homogeneously dispersed between a material and a substrate.

本発明の第２の目的は、上記グラフェン補強銅系複合接点材料の製造方法を提供することにある。   The second object of the present invention is to provide a method for producing the graphene-reinforced copper-based composite contact material.

本発明の第１の目的を達成するための技術的手段は次の通りである。酸化物粉末：０．０１〜１０質量％、炭化物粉末：０．０１〜２質量％、残部：グラフェン被覆銅粉末又はグラフェン被覆銅合金粉末からなり、前記グラフェン被覆の厚さが１０ｎｍ以下である。   Technical means for achieving the first object of the present invention are as follows. Oxide powder: 0.01 to 10% by mass, carbide powder: 0.01 to 2% by mass, balance: graphene-coated copper powder or graphene-coated copper alloy powder, and the thickness of the graphene coating is 10 nm or less.

さらに、酸化物はＳｎＯ２、ＣｕＯ、ＺｎＯ、Ｆｅ２Ｏ３、ＲＥＯの１種又は複数種である。 Furthermore, the oxide is one or more of SnO 2 , CuO, ZnO, Fe 2 O 3 , and REO.

さらに、炭化物はＷＣ、ＶＣ、Ｂ４Ｃなどの１種又は複数種である。 Further, the carbide is one or more of WC, VC, B 4 C and the like.

さらに、銅合金中の銅の含有量が９５％以上であり、該銅合金はＣｕＡｌ、ＣｕＺｎ、ＣｕＮｉ、ＣｕＢ、ＣｕＴｅ、ＣｕＲＥの１種であるか、又は、該銅合金はＣｕと少なくとも２種の他の元素との組み合わせである。   Furthermore, the copper content in the copper alloy is 95% or more, and the copper alloy is one of CuAl, CuZn, CuNi, CuB, CuTe, CuRE, or the copper alloy is at least two kinds of Cu. It is a combination with other elements.

さらに、前記グラフェン被覆銅粉末中、銅粉末の粒子表面に対するグラフェンの被覆率が５０％〜１００％であり、前記グラフェン被覆銅合金粉末中、銅合金粉末の粒子表面に対するグラフェンの被覆率が５０％〜１００％である。   Furthermore, in the graphene-coated copper powder, the graphene coverage on the particle surface of the copper powder is 50% to 100%, and in the graphene-coated copper alloy powder, the graphene coverage on the particle surface of the copper alloy powder is 50%. ~ 100%.

本発明の第２の目的を達成するための技術的手段は次の工程を含む。   The technical means for achieving the second object of the present invention includes the following steps.

（１）化学蒸着法、又は液相酸化グラファイト還元法、又はその他グラフェン成長技術によって、銅粉末又は銅合金粉末の粒子表面をグラフェンで被覆して、グラフェン被覆銅粉末又はグラフェン被覆銅合金粉末を形成するグラフェン被覆銅粉末又はグラフェン被覆銅合金粉末の製造工程、   (1) A graphene-coated copper powder or a graphene-coated copper alloy powder is formed by coating the particle surface of a copper powder or a copper alloy powder with graphene by a chemical vapor deposition method, a liquid phase graphite oxide reduction method, or other graphene growth techniques. Manufacturing process of graphene-coated copper powder or graphene-coated copper alloy powder,

（２）グラフェン被覆銅粉末又はグラフェン被覆銅合金粉末、前記酸化物粉末、前記炭化物粉末を混合、打錠、焼結、押出して、銅系複合接点材料を製造するか、又は混合、成形、焼結、再圧して銅系複合接点材料を製造する工程。   (2) A graphene-coated copper powder or graphene-coated copper alloy powder, the oxide powder, and the carbide powder are mixed, tableted, sintered, and extruded to produce a copper-based composite contact material, or mixed, molded, and sintered. The process of producing a copper-based composite contact material by bonding and re-pressing.

本発明の銅系複合接点材料は、各々の銅又は銅合金粉末が外部に露出しないように、グラフェンで銅又は銅合金の表面を被覆して、銅の酸化を防止し、従来の銅系接点材料では解決できない低温酸化問題を解決した。グラフェンの比表面積が大きいため、アークによる溶融池の粘度が増大し、アーク飛散が低減され、耐アーク消耗性が向上するだけではなく、溶融池内の補強材（炭化物及び酸化物）がグラフェンにより、沈殿又は浮遊による凝集が発生しにくく、接点材料の消耗層の成分均一性が確保されて、接点動作中の接触抵抗の安定性が確保される。   The copper-based composite contact material of the present invention covers the surface of copper or copper alloy with graphene so that each copper or copper alloy powder is not exposed to the outside, thereby preventing the oxidation of copper. The low temperature oxidation problem that cannot be solved by the material was solved. Since the specific surface area of graphene is large, the viscosity of the molten pool due to the arc increases, the arc scattering is reduced, the arc wear resistance is improved, and the reinforcing material (carbide and oxide) in the molten pool is graphene. Aggregation due to precipitation or floating is unlikely to occur, the uniformity of the components of the consumable layer of the contact material is ensured, and the stability of contact resistance during contact operation is ensured.

グラフェンが炭素元素特有の耐溶着性を有するため、銅系材料の耐溶着性を向上させた。グラフェンの高導電性により銅系接点材料の体積抵抗率も低くなった。   Since graphene has the welding resistance peculiar to carbon elements, the welding resistance of the copper-based material is improved. Due to the high conductivity of graphene, the volume resistivity of copper-based contact materials has also been lowered.

本発明の接点材料は、従来の銅系接点よりも優れた耐酸化性及び耐消耗性を有し、低圧遮断器、接触器及び継電器に適用することができる。   The contact material of the present invention has better oxidation resistance and wear resistance than conventional copper-based contacts, and can be applied to low-voltage circuit breakers, contactors, and relays.

次に実施形態により本発明を詳しく説明するが、実施形態は本発明を詳しく説明するためのものであって、本発明の保護範囲を限定するものではない。当業者は上述した発明の内容に基づいて本発明に改良や変更を加えることができる。   Next, the present invention will be described in detail by way of embodiments. However, the embodiments are for explaining the present invention in detail, and do not limit the protection scope of the present invention. Those skilled in the art can make improvements and modifications to the present invention based on the contents of the invention described above.

ＣｕＴｅ／ＧＲＮ ＷＣＳｎＯ２の組成が、ＷＣ：１質量％、ＳｎＯ２：１質量％、残部：厚さ１０ｎｍ以下のグラフェンで被覆されたＣｕＴｅであり、ＣｕＴｅ合金中のＣｕの含有量が９９．５％であり、残りはＴｅである。ＣｕＴｅ合金粉末を噴霧して、酸化グラファイト水分散液を製造し、酸化グラファイト水分散液を銅合金粉末含有ヒドラジン水和物水溶液中で還元させてＣｕＴｅ／ＧＲＮ粉末を製造し、この粉末をＷＣ、ＳｎＯ２粉末と機械混合して、ＣｕＴｅ／ＧＲＮ ＷＣＳｎＯ２混合粉末を製造し、さらに、静水圧圧縮、焼結、押出・緻密化を経て、銅系複合接点材料を製造する。この組成で製造された銅系複合接点材料は密度が８．７８ｇ／ｃｍ３、抵抗率が２．１８μΩ．ｃｍ、硬度がＨＶ１０８である。 The composition of CuTe / GRN WCSnO 2 is CuTe coated with graphene with WC: 1 mass%, SnO 2 : 1 mass% and the balance: 10 nm or less in thickness, and the Cu content in the CuTe alloy is 99.5. % And the rest is Te. A CuTe alloy powder is sprayed to produce a graphite oxide aqueous dispersion, and the graphite oxide aqueous dispersion is reduced in a copper alloy powder-containing hydrazine hydrate aqueous solution to produce a CuTe / GRN powder. A CuTe / GRN WCSnO 2 mixed powder is manufactured by mechanical mixing with SnO 2 powder, and a copper-based composite contact material is manufactured through isostatic pressing, sintering, extrusion and densification. The copper-based composite contact material manufactured with this composition has a density of 8.78 g / cm 3 and a resistivity of 2.18 μΩ. cm and hardness is HV108.

Ｃｕ／ＧＲＮ Ｂ４ＣＳｎＯ２の組成が、ＢＣ：０．５質量％、ＳｎＯ２：０．３質量％、残部：厚さ１０ｎｍ以下のグラフェンで被覆されたＣｕである。Ｃｕ粉末を製造し、管状化学蒸着炉内でＣｕ粉末をグラフェンで被覆し（メタン雰囲気）、Ｃｕ／ＧＲＮ粉末を破砕した後、Ｂ４Ｃ粉末、ＳｎＯ２粉末と機械混合し、その後静水圧圧縮、焼結、押出を経て緻密化された銅系複合接点材料を製造する。この組成で製造された銅系複合接点材料は密度が８．７２ｇ／ｃｍ３、抵抗率が２．０６μΩ．ｃｍ、硬度がＨＶ９３．５である。 The composition of Cu / GRN B 4 CSnO 2 is Cu coated with graphene with BC: 0.5 mass%, SnO 2 : 0.3 mass%, and the balance: 10 nm or less in thickness. Cu powder is manufactured, coated with graphene in a tubular chemical vapor deposition furnace (methane atmosphere), Cu / GRN powder is crushed, then mechanically mixed with B 4 C powder and SnO 2 powder, and then hydrostatically compressed A copper-based composite contact material is manufactured through sintering, extrusion, and densification. The copper-based composite contact material produced with this composition has a density of 8.72 g / cm 3 and a resistivity of 2.06 μΩ. cm and hardness is HV93.5.

本発明は上記の実施例に限定されるものではない。   The present invention is not limited to the above embodiments.

Claims (4)

酸化物粉末：０．０１〜１０質量％、炭化物粉末：０．０１〜２質量％、残部：グラフェン被覆銅粉末又はグラフェン被覆銅合金粉末からなり、
前記酸化物が、ＳｎＯ２、ＣｕＯ、ＺｎＯ、Ｆｅ２Ｏ３、ＲＥＯの１種又は複数種であり、
前記炭化物が、炭化タングステン、炭化バナジウム、炭化ホウ素の１種又は複数種であり、
前記グラフェン被覆の厚さが１０ｎｍ以下であることを特徴とするグラフェン補強銅系複合接点材料。 Oxide powder: 0.01 to 10% by mass, carbide powder: 0.01 to 2% by mass, balance: graphene-coated copper powder or graphene-coated copper alloy powder,
The oxide is one or more of SnO 2 , CuO, ZnO, Fe 2 O 3 , REO,
The carbide is one or more of tungsten carbide, vanadium carbide, boron carbide,
A graphene-reinforced copper-based composite contact material, wherein the graphene coating has a thickness of 10 nm or less. 銅合金中の銅の含有量が９５％以上であり、銅合金がＣｕＡｌ、ＣｕＺｎ、ＣｕＮｉ、ＣｕＢ、ＣｕＴｅ、ＣｕＲＥの１種であるか、又は、該銅合金がＣｕと少なくとも２種の他の元素との組み合わせであることを特徴とする請求項１に記載のグラフェン補強銅系複合接点材料。   The copper content in the copper alloy is 95% or more, and the copper alloy is one of CuAl, CuZn, CuNi, CuB, CuTe, CuRE, or the copper alloy is Cu and at least two other kinds The graphene-reinforced copper-based composite contact material according to claim 1, which is a combination with an element. 前記グラフェン被覆銅粉末中、銅粉末の粒子表面に対するグラフェンの被覆率が５０％〜１００％であり、
前記グラフェン被覆銅合金粉末中、銅合金粉末の粒子表面に対するグラフェンの被覆率が５０％〜１００％であることを特徴とする請求項１に記載のグラフェン補強銅系複合接点材料。 In the graphene-coated copper powder, the coverage of graphene with respect to the particle surface of the copper powder is 50% to 100%,
2. The graphene-reinforced copper-based composite contact material according to claim 1, wherein in the graphene-coated copper alloy powder, the graphene coverage with respect to the particle surface of the copper alloy powder is 50% to 100%. （１）化学蒸着法又は液相酸化グラファイト還元法で、銅粉末又は銅合金粉末の粒子表面をグラフェンで被覆して、グラフェン被覆銅粉末又はグラフェン被覆銅合金粉末を形成するグラフェン被覆銅粉末又はグラフェン被覆銅合金粉末の製造工程と、
（２）グラフェン被覆銅粉末又はグラフェン被覆銅合金粉末、前記酸化物粉末、前記炭化物粉末を混合、打錠、焼結、押出して、銅系複合接点材料を製造するか、又は混合、 成形、焼結、再圧して銅系複合接点材料を製造する工程と、を含むことを特徴とする請求項１に記載のグラフェン補強銅系複合接点材料の製造方法。 (1) A graphene-coated copper powder or graphene that forms a graphene-coated copper powder or a graphene-coated copper alloy powder by coating the particle surface of a copper powder or a copper alloy powder with graphene by a chemical vapor deposition method or a liquid phase graphite oxide reduction method Manufacturing process of coated copper alloy powder;
(2) A graphene-coated copper powder or graphene-coated copper alloy powder, the oxide powder, and the carbide powder are mixed, tableted, sintered, and extruded to produce a copper-based composite contact material, or mixed, molded, and sintered. The method for producing a graphene-reinforced copper-based composite contact material according to claim 1, further comprising a step of producing a copper-based composite contact material by bonding and re-pressing.
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