JP2012132034A - Metal material having hollow structure, metal particle and its manufacturing method - Google Patents
Metal material having hollow structure, metal particle and its manufacturing method Download PDFInfo
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- 239000007769 metal material Substances 0.000 title claims abstract description 26
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- 239000002923 metal particle Substances 0.000 title claims description 26
- 239000002184 metal Substances 0.000 claims abstract description 75
- 229910052751 metal Inorganic materials 0.000 claims abstract description 75
- 239000002245 particle Substances 0.000 claims abstract description 59
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000007787 solid Substances 0.000 claims description 6
- 239000000843 powder Substances 0.000 abstract description 12
- 238000002844 melting Methods 0.000 abstract description 11
- 230000008018 melting Effects 0.000 abstract description 11
- 239000002861 polymer material Substances 0.000 abstract description 7
- 239000011162 core material Substances 0.000 abstract description 5
- 238000005266 casting Methods 0.000 abstract description 3
- 238000005187 foaming Methods 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 abstract description 2
- 229910001361 White metal Inorganic materials 0.000 description 16
- 239000010969 white metal Substances 0.000 description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 15
- 238000004898 kneading Methods 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 9
- 239000003094 microcapsule Substances 0.000 description 9
- 238000001816 cooling Methods 0.000 description 8
- 238000000879 optical micrograph Methods 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 229910045601 alloy Inorganic materials 0.000 description 7
- 239000000956 alloy Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000000377 silicon dioxide Substances 0.000 description 7
- 229920000877 Melamine resin Polymers 0.000 description 6
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 6
- 239000000155 melt Substances 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 239000010419 fine particle Substances 0.000 description 4
- 239000006260 foam Substances 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 239000011163 secondary particle Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000005484 gravity Effects 0.000 description 3
- 239000011368 organic material Substances 0.000 description 3
- 125000006850 spacer group Chemical group 0.000 description 3
- 239000002562 thickening agent Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000013016 damping Methods 0.000 description 2
- 239000004088 foaming agent Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000001939 inductive effect Effects 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002667 nucleating agent Substances 0.000 description 2
- 229920000620 organic polymer Polymers 0.000 description 2
- 230000000379 polymerizing effect Effects 0.000 description 2
- 235000019353 potassium silicate Nutrition 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004552 water soluble powder Substances 0.000 description 2
- 229920003169 water-soluble polymer Polymers 0.000 description 2
- 229910007116 SnPb Inorganic materials 0.000 description 1
- 241001062472 Stokellia anisodon Species 0.000 description 1
- 229910000711 U alloy Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011246 composite particle Substances 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- -1 fluororesin Substances 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
Description
本発明は、中空構造を有する粒子を使用して製造した中空構造を有する金属材料、金属粒子およびその製造方法に関するものである。 The present invention relates to a metal material having a hollow structure produced using particles having a hollow structure, a metal particle, and a method for producing the metal material.
内部が気体の中空構造を有する金属材料は、中空構造を持たない材料に比べて密度が低く、熱や音の伝達を抑制する構造を持つため、自動車などのエネルギー削減につながる高強度・低比重の構造部材や、音響特性・伝熱特性を制御可能な構造部材などに用いられる。また内部に中空構造を含有する金属粒子は、中空構造を持たない材料にくらべて密度が低いため、粒子の沈降が問題となるMR（Magneto-Rheological）粒子やER（Electro−Rheological）粒子などに期待されている。本申請での金属粒子は外部体積の等価直径５ｍｍ以下の金属構造体と定義する。 Metal materials with a hollow structure inside the gas have a lower density than materials without a hollow structure and have a structure that suppresses the transmission of heat and sound. And structural members capable of controlling acoustic characteristics and heat transfer characteristics. Also, metal particles containing a hollow structure inside have a lower density than materials that do not have a hollow structure. Therefore, such as MR (Magneto-Rheological) particles and ER (Electro-Rheological) particles, where particle sedimentation is a problem. Expected. The metal particle in this application is defined as a metal structure having an outer volume equivalent diameter of 5 mm or less.
従来の中空構造を有する金属材料の製法としては、大きく分けて溶融時に増粘剤と発泡核剤を用いて溶融金属中に発泡核剤由来の中空構造を作る鋳造法（非特許文献１）、あるいは金属粉末に高分子材料を混ぜて成型する粉末焼結法（非特許文献２）がある。 As a conventional method for producing a metal material having a hollow structure, a casting method (Non-patent Document 1) for creating a hollow structure derived from a foam nucleating agent in a molten metal using a thickener and a foam nucleating agent at the time of melting. Alternatively, there is a powder sintering method (Non-patent Document 2) in which a polymer material is mixed with metal powder and molded.
鋳造法としては、金属を加熱して溶融させた後、温度を下げて溶融金属に粘性を付与したあと発泡剤を添加して、発泡反応状態にある発泡溶融金属を成形する方法（特許文献１）、溶融金属に増粘剤を添加して攪拌し、これに発泡剤を添加し、鋳型内で発泡充満させてから急冷する方法（特許文献２）がある。 As a casting method, after a metal is heated and melted, the temperature is lowered to give viscosity to the molten metal, and then a foaming agent is added to form a foamed molten metal in a foaming reaction state (Patent Document 1). There is a method (Patent Document 2) in which a thickener is added to a molten metal and stirred, a foaming agent is added to the molten metal, the foam is filled in a mold, and then rapidly cooled.
粉末焼結法としては、金属粉末、バインダ、水溶性粉末および水溶性高分子材料を混練し、水によって水溶性粉末及び水溶性高分子材料を抽出、除去後、焼成することにより、金属多孔体を得る方法（特許文献３）、ポアの空間をスペーサー材料によって確保して、金属とスペーサーを圧縮成型したあと、スペーサーを除去することにより、ポーラス金属材料を製造する方法（特許文献４）、多孔質の有機高分子材料を分散剤含有水溶液と金属粉末を混合した液に含浸し、乾燥後非酸化性ガス雰囲気中で加熱することにより有機高分子材料を脱脂し更に原料粉末を焼結する方法（特許文献５）などがある。 As the powder sintering method, a metal porous body is obtained by kneading metal powder, a binder, a water-soluble powder and a water-soluble polymer material, extracting the water-soluble powder and the water-soluble polymer material with water, removing it, and firing it. (Patent Document 3), a method of producing a porous metal material by securing the pore space with a spacer material, compression molding the metal and the spacer, and then removing the spacer (Patent Document 4), porous Of high-quality organic polymer material impregnated with a mixture of a dispersant-containing aqueous solution and metal powder, followed by drying and heating in a non-oxidizing gas atmosphere to degrease the organic polymer material and further sinter the raw material powder (Patent Document 5).
また、粒子を用いて多孔質材料を作り出す手法としては、水を内包するマイクロカプセルを金属アルコキシドと共存させ、加水分解反応により多孔質セラミックスを製造する方法などがある（特許文献６参照）。 In addition, as a method for producing a porous material using particles, there is a method in which a microcapsule enclosing water coexists with a metal alkoxide, and a porous ceramic is produced by a hydrolysis reaction (see Patent Document 6).
また、中空の粒子を作り出す手法としては、気泡の表面において液相中の物質同士を重合させて固体膜を生み出して中空粒子化する方法（特許文献７、非特許文献３）、有機材料のコア微粒子を金属化合物によって被覆した複合粒子を作成した後、空気または酸素存在下で加熱することにより、コア微粒子の有機材料を分解ガス化させて粒子内部に空孔をもたせる方法（特許文献８、９）などがある。 Moreover, as a method of creating hollow particles, a method of polymerizing substances in a liquid phase on the surface of a bubble to produce a solid film to form hollow particles (Patent Document 7, Non-Patent Document 3), an organic material core A method of producing composite particles in which fine particles are coated with a metal compound and then heating them in the presence of air or oxygen to decompose and gasify the organic material of the core fine particles to have pores inside the particles (Patent Documents 8 and 9). )and so on.
前記の背景技術において、溶融時に増粘剤と発泡核材を用いる方法は、溶融金属の粘度向上のために添加元素を加えるため、セル形態が制御できないこと、中空構造のサイズも数ミリオーダーと大きくなってしまうことが問題である。 In the above-mentioned background art, the method of using a thickener and a foam core material at the time of melting adds an additive element for improving the viscosity of the molten metal, so that the cell form cannot be controlled, and the size of the hollow structure is also on the order of several millimeters. The problem is that it grows.
前記の背景技術における金属粉末に高分子材料を混ぜ成型する方法は、金属粉末作成が困難・危険であること、大型成型品の作製が困難であることが問題である。 The method of mixing and molding a polymer material with metal powder in the background art has problems that it is difficult and dangerous to produce metal powder and that it is difficult to produce a large molded product.
前記の背景技術におけるマイクロカプセルを利用した多孔質セラミックスの製造方法は、内部に水が入った中実構造のマイクロカプセルを用いており、直接中空構造を生み出せないこととセラミックスを対象としており金属での作成例がないことが問題である。 The method for producing porous ceramics using microcapsules in the background art described above uses solid microcapsules with water inside, and cannot directly create a hollow structure. There is a problem that there is no example of creation.
前記の背景技術におけるコア微粒子の有機材料を分解ガス化させて粒子内部に空孔をもたせる方法は、気化した樹脂を除去する行程が必要となり工程が複雑化する上、独立した中空構造ができにくいことが問題である。 The method of decomposing and gasifying the organic material of the core fine particles in the background art described above to have pores inside the particles requires a process of removing the vaporized resin, complicates the process, and makes it difficult to form an independent hollow structure. That is a problem.
また、前記の背景技術における気泡の表面において液相中の物質同士を重合させて固体膜を生み出して中空粒子化する方法は、十分な耐熱性および耐久性を有しておらず、中空構造が容易に破損してしまうことが問題である。 In addition, the method of polymerizing substances in the liquid phase on the surface of the bubble in the background art to produce a solid film to form hollow particles does not have sufficient heat resistance and durability, and the hollow structure The problem is that it easily breaks.
本発明は、中空構造を有する固体粒子を用いることで、前記の従来の中空構造を有する金属あるいは金属粒子が有する問題を解決することを課題としている。 This invention makes it a subject to solve the problem which the metal or metal particle which has the said conventional hollow structure by using the solid particle which has a hollow structure.
本発明における中空構造を有する粒子を使用して製造した中空構造を有する金属材料、金属粒子およびその製造方法では、溶融状態にある金属に、中空構造を有する粒子を混錬・分散後、固化させることにより、中空構造を有した金属材料または金属粒子が生成する。 In the metal material having a hollow structure produced using the particles having a hollow structure in the present invention, the metal particles, and the production method thereof, the particles having the hollow structure are solidified after being kneaded and dispersed in the molten metal. As a result, a metal material or metal particles having a hollow structure is generated.
本発明に係る中空構造を有する粒子を使用して製造した中空構造を有する金属材料、金属粒子およびその製造方法によって以下の効果を得ることができる。
（１）中空構造を有し金属の融点以上もしくは同等の融点を持つ粒子を添加すれば混錬工程のみで、簡便に金属材料または金属粒子中に中空構造を付与することができる。
（２）分級操作などにより中空構造を有する粒子の径や比重を制御することで、金属材料または金属粒子の中空構造の径、形状、比重を容易に変えることができる。
（３）金属中に中空構造を付与することができるため、音や熱の伝達を抑制することができる。
The following effects can be obtained by the metal material having a hollow structure produced using the particles having a hollow structure according to the present invention, the metal particles, and the production method thereof.
(1) If particles having a hollow structure and having a melting point equal to or higher than the melting point of the metal are added, the hollow structure can be easily provided in the metal material or metal particles only by the kneading step.
(2) The diameter, shape, and specific gravity of the hollow structure of the metal material or metal particles can be easily changed by controlling the diameter and specific gravity of the particles having a hollow structure by classification operation or the like.
(3) Since a hollow structure can be provided in the metal, transmission of sound and heat can be suppressed.
本発明における中空構造を有する金属材料または金属粒子の製造方法では、溶融状態の金属中に中空構造を有する粒子を添加して混錬後、固化させることによって中空構造を有する金属材料または金属粒子が生成する。以下、本発明を実施するための最良の形態について図１を参照して説明する。 In the method for producing a metal material or metal particle having a hollow structure in the present invention, the metal material or metal particle having a hollow structure is obtained by adding particles having a hollow structure to a molten metal and kneading and then solidifying. Generate. Hereinafter, the best mode for carrying out the present invention will be described with reference to FIG.
本発明を実施するための最良の形態では、容器１に金属２と中空構造を有する粒子３をいれ、加熱手段４によって金属２を溶融させたあと、混錬手段５によって、中空構造を有する粒子３は金属２の溶融体中に分散される。中空構造を有する粒子３の分散後、冷却手段６によって溶融状態の金属２を固化させることによって、中空構造を有する金属材料または金属粒子７が生成する。 In the best mode for carrying out the present invention, a metal 2 and particles 3 having a hollow structure are placed in a container 1, the metal 2 is melted by heating means 4, and then particles having a hollow structure are mixed by kneading means 5. 3 is dispersed in the melt of metal 2. After the particles 3 having a hollow structure are dispersed, the metal 2 in the molten state is solidified by the cooling means 6 to produce a metal material or metal particles 7 having a hollow structure.
前記容器１については、溶融させる金属２の融点以上で安定に形状を保持できるものであれば特に限定されるものではないが、アルミナ、石英、フッ素樹脂、ニッケル、ステンレス製のるつぼなどが例示される。 The container 1 is not particularly limited as long as the shape can be stably maintained above the melting point of the metal 2 to be melted, but examples thereof include alumina, quartz, fluororesin, nickel, and a stainless steel crucible. The
前記金属２の種類については、加熱手段によって溶融状態に相変化する材料であれば特に限定されるものではないが、中空構造を有する粒子４の添加および混錬による分散を容易に行うために、融点８００℃以下の金属が好ましく、ＳｎＳｂＣｕ合金、ＳｎＰｂ合金、ＳｎＰｂＣｄ合金、ＳｎＢｉＣｄ合金、ＳｎＢｉ合金、より具体的には、ホワイトメタル（ＳｎＳｂＣｕ合金）やUアロイ（ＳｎＢｉ合金）が例示される。 The type of the metal 2 is not particularly limited as long as it is a material that changes in a molten state by a heating means, but in order to easily disperse by addition and kneading of the particles 4 having a hollow structure, A metal having a melting point of 800 ° C. or lower is preferable, and examples thereof include SnSbCu alloy, SnPb alloy, SnPbCd alloy, SnBiCd alloy, SnBi alloy, and more specifically, white metal (SnSbCu alloy) and U alloy (SnBi alloy).
前記中空構造を有する粒子３については、中空構造を有し、溶融した金属２中に添加するまで粒子形状を維持できる粒子であれば、特に限定されるものではないが、混錬の容易性や中空構造の優位性の観点から、直径は５mm以下、粒子の体積に対して１０％以上の中空構造を有する粒子が好ましい。また、中空構造を有する粒子３が形状を保つことができる耐熱温度については、金属２の溶融体中に微細な気泡を分散できれば溶融金属中に中空構造が形成されるため、瞬時に粒子が溶解しなければ特に限定されるものではないが、金属２中で１秒以上形状を保持できることが好ましく、より好ましくは粒子の融点が金属２の融点以上であることが望ましい。具体的な中空構造を有する粒子としてはメラミン中空マイクロカプセル（特許文献７）、シリカ中空粒子（Glassbubbles、スリーエム）、などが例示される。また、本手法で生成される中空構造を有する金属粒子を、中空構造を有する金属材料を生み出す粒子として使用することも好適な例として挙げられる。 The particles 3 having the hollow structure are not particularly limited as long as the particles have a hollow structure and can maintain the particle shape until they are added to the molten metal 2. From the viewpoint of the superiority of the hollow structure, particles having a hollow structure with a diameter of 5 mm or less and 10% or more with respect to the volume of the particles are preferable. In addition, regarding the heat resistance temperature at which the particles 3 having a hollow structure can be maintained in shape, if fine bubbles can be dispersed in the melt of the metal 2, a hollow structure is formed in the molten metal, so that the particles dissolve instantaneously. Otherwise, there is no particular limitation, but it is preferable that the shape can be maintained in the metal 2 for 1 second or longer, and more preferably, the melting point of the particles is higher than the melting point of the metal 2. Specific particles having a hollow structure include melamine hollow microcapsules (Patent Document 7), silica hollow particles (Glassbubbles, 3M), and the like. Moreover, it is also mentioned as a suitable example that the metal particle which has the hollow structure produced | generated by this method is used as a particle which produces the metal material which has a hollow structure.
本発明における容器１に入れる金属２に対する中空構造を有する粒子３の体積比が大きい場合、図２に示すような金属２の溶融体の外部および内部に中空構造を有する粒子３が付着した２次粒子が形成する。前記２次粒子中の金属２の溶融体が混錬中の環境温度あるいは冷却手段６によって固化させることによって、中空構造を有する金属粒子が生成する。中空構造を生み出す際の前記金属２に対する中空構造を有する粒子３の体積比については、中空構造を有する粒子３が金属２の液滴に少なくとも一部が付着あるいは内包されればよく、特に指定されるものではないが、中空構造を有する金属粒子を生み出す際には、金属２の体積に対し５０％以上、より好ましくは３００％以上の体積の中空構造を有する粒子３を入れることが望ましい。また、本手法によって形成する中空構造を有する粒子の最小径については、中空構造を有する粒子３の大きさに依存して小さくなるため、中空構造を有する粒子３の大きさは直径１ｍｍ以下、より好ましくは１００μｍ以下であることが望ましい。 When the volume ratio of the particles 3 having a hollow structure to the metal 2 put in the container 1 in the present invention is large, the secondary particles 3 having the hollow structure adhered to the outside and the inside of the melt of the metal 2 as shown in FIG. Particles form. When the melt of the metal 2 in the secondary particles is solidified by the ambient temperature during the kneading or the cooling means 6, metal particles having a hollow structure are generated. The volume ratio of the particles 3 having a hollow structure with respect to the metal 2 when creating the hollow structure is not particularly limited as long as at least a part of the particles 3 having the hollow structure is attached to or included in the droplets of the metal 2. However, when producing metal particles having a hollow structure, it is desirable to put particles 3 having a hollow structure having a volume of 50% or more, more preferably 300% or more, relative to the volume of metal 2. Further, since the minimum diameter of the particles having a hollow structure formed by this method is small depending on the size of the particles 3 having a hollow structure, the size of the particles 3 having a hollow structure is 1 mm or less in diameter. Preferably it is 100 μm or less.
前記加熱手段４については、金属の溶融に用いられる既知の加熱手段を用いれば特に限定されず、好ましくは、電気加熱炉、オイルバス、ホットプレートスターラーなどが例示される。 The heating unit 4 is not particularly limited as long as a known heating unit used for melting a metal is used, and an electric heating furnace, an oil bath, a hot plate stirrer and the like are preferable.
前記混錬手段５については、金属２の溶融体中に中空構造を有する粒子３を分散させることができれば、特に限定されるものではないが、攪拌棒、ホモジナイザー、押出混錬による混錬などが例示される。また、混錬を行う際に、金属が溶融状態を保つことができれば、混錬中の加熱手段４の使用は必須ではない。 The kneading means 5 is not particularly limited as long as the particles 3 having a hollow structure can be dispersed in the melt of the metal 2, but a kneading rod, a homogenizer, extrusion kneading, or the like may be used. Illustrated. In addition, when kneading, if the metal can be kept in a molten state, the use of the heating means 4 during kneading is not essential.
前記冷却手段６については、溶融状態にある金属２を融点以下に下げることができれば特に制限はないが、速やかに冷却する際には、水による冷却、低温恒温器による冷却が例示される。また、常温・常圧で金属が固化する場合には、冷却手段は必須ではない。 The cooling means 6 is not particularly limited as long as the molten metal 2 can be lowered to the melting point or lower. However, when rapidly cooling, cooling with water and cooling with a low-temperature incubator are exemplified. Further, when the metal is solidified at normal temperature and normal pressure, the cooling means is not essential.
以下、本発明を実施例に基づき更に説明するが、本発明はこれに限定されるものではない。 EXAMPLES Hereinafter, although this invention is further demonstrated based on an Example, this invention is not limited to this.
ホワイトメタル２５ｍｌを３０ｍｌのアルミナるつぼにいれ、４００℃に設定した電気炉によって十分加熱し、ホワイトメタルを溶融状態にする。前記溶融金属に水ガラスでコーティングした平均径１００μｍで内部がほぼ空洞（膜厚１μｍ以下）のメラミン中空マイクロカプセル（特許文献７）を５ｍｌ添加し、ステンレス製の攪拌棒によって約６０ｒｐｍで１５分間混錬する。攪拌棒を引き抜き、室温で静置すると溶融状態のホワイトメタルが固化し、内部に中空構造を有する金属が生成する。実施例１によって生成した金属の断面の光学顕微鏡画像を図３に示す。図３に示すように金属内部に大きさ１００〜５００μｍ程度の空洞が確認できることから、メラミン中空マイクロカプセルの空洞に由来する中空構造を有する金属の作成が確認された。 25 ml of white metal is placed in a 30 ml alumina crucible and heated sufficiently by an electric furnace set at 400 ° C. to bring the white metal into a molten state. 5 ml of melamine hollow microcapsules (Patent Document 7) having an average diameter of 100 μm coated with water glass and approximately hollow inside (film thickness of 1 μm or less) were added to the molten metal and mixed for 15 minutes at about 60 rpm with a stainless steel stirring rod. Smelt. When the stirring bar is pulled out and allowed to stand at room temperature, the molten white metal is solidified, and a metal having a hollow structure is generated inside. The optical microscope image of the cross section of the metal produced | generated by Example 1 is shown in FIG. As shown in FIG. 3, since a cavity having a size of about 100 to 500 μm can be confirmed inside the metal, it was confirmed that a metal having a hollow structure derived from the cavity of the melamine hollow microcapsule was produced.
ホワイトメタル１５ｍｌ、前記溶融金属に水ガラスでコーティングした平均径１００μｍで内部がほぼ空洞（膜厚１μｍ以下）のメラミン中空マイクロカプセル（特許文献７）１５ｍｌを３０ｍｌのアルミナるつぼにいれ、４００℃に設定した電気炉によって十分加熱し、ホワイトメタルを溶融状態にする。溶融状態のホワイトメタルとメラミン中空マイクロカプセルが入ったるつぼをステンレス製の攪拌棒によって約６０ｒｐｍで１５分間混錬する。攪拌棒を引き抜き、室温で静置すると溶融状態のホワイトメタルが固化し、内部に中空構造を有する金属が生成する。実施例２によって生成した金属の断面の光学顕微鏡画像を図４に示す。図４に示すように金属内部に大きさ１００〜５００μｍ程度の空洞が確認できることから、メラミン中空マイクロカプセルの空洞に由来する中空構造を有する金属の作成が確認された。また、実施例１（図３）に比べて実施例２（図４）の金属断面中に見られる中空構造の頻度が大きいことから、中空構造を有する粒子の投入量によって、金属材料中に有する中空構造の量を変化させることが可能であることを確認した。 15 ml of white metal, 15 ml of melamine hollow microcapsules (patent document 7) with an average diameter of 100 μm coated with water glass on the molten metal and a hollow inside (film thickness of 1 μm or less) (Patent Document 7) are set at 400 ° C. The white metal is brought into a molten state by sufficiently heating with an electric furnace. A crucible containing molten white metal and melamine hollow microcapsules is kneaded with a stainless steel stirring rod at about 60 rpm for 15 minutes. When the stirring bar is pulled out and allowed to stand at room temperature, the molten white metal is solidified, and a metal having a hollow structure is generated inside. The optical microscope image of the cross section of the metal produced | generated by Example 2 is shown in FIG. As shown in FIG. 4, since a cavity having a size of about 100 to 500 μm can be confirmed inside the metal, it was confirmed that a metal having a hollow structure derived from the cavity of the melamine hollow microcapsule was produced. Moreover, since the frequency of the hollow structure seen in the metal cross section of Example 2 (FIG. 4) is larger than that of Example 1 (FIG. 3), it is contained in the metal material depending on the amount of particles having the hollow structure. It was confirmed that the amount of the hollow structure can be changed.
ホワイトメタル１０ｍｌ、平均径１６μｍで内部に直径約１４μｍの空洞を持つシリカ中空粒子（Glassbubbles ｉＭ３０Ｋ、スリーエム）２０ｍｌを３０ｍｌのアルミナるつぼにいれ、４００℃に設定した電気炉によって十分加熱し、ホワイトメタルを溶融状態にする。溶融状態のホワイトメタルとシリカ中空粒子が入ったるつぼをステンレス製の攪拌棒によって約６０ｒｐｍで１５分間混錬する。本実施例では、シリカ中空粒子の量が多いため、溶融状態のホワイトメタルが中空粒子によって包まれたパウダー状の２次粒子が生成する。攪拌棒を引き抜き、室温で静置すると溶融状態のホワイトメタルが固化し、表面および内部に中空構造を有する直径２０μｍから５ｍｍの金属粒子が生成する。実施例３によって生成した金属粒子の光学顕微鏡画像を図５に示す。図５に示すように金属表面に１０〜２０μｍの中空粒子が付着した直径約５００μｍの粒子が確認できることから、金属表面にシリカ中空粒子内部の空洞に由来する中空構造を有する金属粒子の作成が確認された。 10 ml of white metal, 20 ml of silica hollow particles (Glassbubbles iM30K, 3M) with an average diameter of 16 μm and a cavity of about 14 μm inside are placed in a 30 ml alumina crucible and heated sufficiently by an electric furnace set at 400 ° C. Bring to a molten state. A crucible containing molten white metal and silica hollow particles is kneaded with a stainless steel stirring rod at about 60 rpm for 15 minutes. In this example, since the amount of silica hollow particles is large, powdery secondary particles in which a molten white metal is wrapped with hollow particles are generated. When the stirring bar is pulled out and allowed to stand at room temperature, the molten white metal is solidified, and metal particles with a diameter of 20 μm to 5 mm having a hollow structure on the surface and inside are generated. An optical microscope image of the metal particles produced in Example 3 is shown in FIG. As shown in FIG. 5, since particles having a diameter of about 500 μm with 10-20 μm hollow particles adhering to the metal surface can be confirmed, the creation of metal particles having a hollow structure derived from the cavity inside the silica hollow particles is confirmed on the metal surface. It was done.
実施例３によって作成した中空構造を有する金属粒子２０ｍｌを３０ｍｌのアルミナるつぼにいれ、更にるつぼにホワイトメタルを１０ｍｌ追加し再度４００℃に設定した電気炉によって十分加熱する。追加したホワイトメタルが溶融状態になった後、溶融状態のホワイトメタルとシリカ中空粒子が入ったるつぼをステンレス製の攪拌棒によって約６０ｒｐｍで１５分間混錬する。攪拌棒を引き抜き、室温で静置すると溶融状態のホワイトメタルが固化し、内部に中空構造を有する金属が生成する。実施例４によって生成した金属の断面の光学顕微鏡画像を図６に示す。図６に示すように金属内部に環状で外形が約１ｍｍ程度の空洞が確認できることから、実施例３で生成した中空構造を有する金属微粒子の外周に付着したシリカ中空粒子の空洞に由来する中空構造を有する金属の作成が確認された。 20 ml of the metal particles having a hollow structure prepared according to Example 3 are placed in a 30 ml alumina crucible, and 10 ml of white metal is further added to the crucible, and the mixture is sufficiently heated by an electric furnace set at 400 ° C. again. After the added white metal is in a molten state, the crucible containing the molten white metal and silica hollow particles is kneaded with a stainless steel stirring rod at about 60 rpm for 15 minutes. When the stirring bar is pulled out and allowed to stand at room temperature, the molten white metal is solidified, and a metal having a hollow structure is generated inside. The optical microscope image of the cross section of the metal produced | generated by Example 4 is shown in FIG. As shown in FIG. 6, a hollow structure having an annular shape and an outer shape of about 1 mm can be confirmed inside the metal, so that the hollow structure is derived from the hollow of silica hollow particles attached to the outer periphery of the metal fine particles having the hollow structure generated in Example 3. The creation of a metal with
実施例４で生成した金属にパルスレーザによって広帯域の超音波を誘起して超音波伝播特性を測定した結果を図７に示す。図７では、比較対象の中空構造を持たない金属に比べて実施例４で生成した金属では、金属に伝わる振動の高周波成分が全てカットされていることを示しており、固有の特性を有していることが確認できる。 FIG. 7 shows the result of measuring ultrasonic propagation characteristics by inducing broadband ultrasonic waves to the metal produced in Example 4 using a pulse laser. FIG. 7 shows that the high-frequency component of vibration transmitted to the metal is all cut in the metal produced in Example 4 as compared with the metal having no hollow structure for comparison, and has a unique characteristic. Can be confirmed.
なお、以上の説明は、例示したものであり、本発明は前記実施例に限定されるものではない。 In addition, the above description is an illustration and this invention is not limited to the said Example.
本発明で得られる中空構造を有する金属材料は高強度・軽量・高減衰特性素材であるため、衝撃緩衝部材や減衰材料などへの応用が期待される。また、本発明で得られる中空構造を有する金属粒子は金属材料でありながら付着あるいは内包する中空粒子の量に応じて、比重を調整することができるため、粒子の沈降が問題とされるMR（Magneto-Rheological）粒子やER（Electro−Rheological）粒子などへの応用が期待される。 Since the metal material having a hollow structure obtained by the present invention is a material having high strength, light weight, and high damping characteristics, it is expected to be applied to shock absorbing members, damping materials, and the like. In addition, the metal particles having a hollow structure obtained by the present invention can adjust the specific gravity according to the amount of the hollow particles to be attached or encapsulated while being a metal material. Application to Magneto-Rheological) particles and ER (Electro-Rheological) particles is expected.
１ 容器
２ 金属
３ 中空構造を有する粒子
４ 加熱手段
５ 混錬手段
６ 冷却手段
７ 中空構造を有する金属材料または金属粒子
DESCRIPTION OF SYMBOLS 1 Container 2 Metal 3 Particle | grains which have a hollow structure 4 Heating means 5 Kneading means 6 Cooling means 7 Metal material or metal particle which has a hollow structure
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| EP3650144A1 (en) * | 2018-11-02 | 2020-05-13 | Toyota Jidosha Kabushiki Kaisha | Method for producing metal structure |
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