JP2011073113A - Double-coated diamond abrasive particle and method of manufacturing the same - Google Patents
Double-coated diamond abrasive particle and method of manufacturing the same Download PDFInfo
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本発明は、二重被覆ダイヤモンド研磨材粒子、特に放熱性に優れたダイヤモンド研磨材粒子及びその製造方法に関する。 The present invention relates to double-coated diamond abrasive particles, particularly diamond abrasive particles excellent in heat dissipation and a method for producing the same.
ダイヤモンド粒子を用いた工具の製作、特に結合剤として金属を用いる工具の製作に際し、ボンド材による保持力の向上を目的として、粒子表面に金属炭化物膜を形成する技術が知られている。
これは結合剤金属に対する濡れ性(化学反応性)が、ダイヤモンド(炭素)よりも金属炭化物の方が良好であることに基づいている。しかもダイヤモンド粒子表面を覆っている金属炭化物の炭素は、ダイヤモンド粒子から供給されることから、粒子表面と金属炭化物とは連続しており、結果としてダイヤモンド粒子が金属炭化物層を介した化学結合によって結合剤金属中に固定されることとなる。 This is based on the fact that metal carbides have better wettability (chemical reactivity) to the binder metal than diamond (carbon). Moreover, since the carbon of the metal carbide covering the surface of the diamond particle is supplied from the diamond particle, the particle surface and the metal carbide are continuous. As a result, the diamond particle is bonded by a chemical bond through the metal carbide layer. It will be fixed in the agent metal.
ダイヤモンド粒子表面に金属炭化物膜を形成する技術としては、蒸着、スパッタリング、ＣＶＤなどの手法が知られており、加熱下で粒子表面に生成された金属とダイヤモンドとの反応によって、炭化物が形成される。 Known techniques for forming a metal carbide film on the surface of diamond particles include vapor deposition, sputtering, CVD, and the like, and a carbide is formed by the reaction between diamond and metal generated on the particle surface under heating. .
一方、より簡単に金属炭化物膜を形成する技術としてパイロゾル法が知られている。これは金属イオンを含む溶融塩中にダイヤモンド粒子を浸漬させて、金属イオンとダイヤモンドとの反応により粒子表面に炭化物被覆を形成させる方法であって、融液中における反応であることから、粒子表面全面にほぼ均一な厚さの被覆を容易に形成でき、またサブミクロン級の粒子表面にも被覆形成が可能という特徴を有する。 On the other hand, a pyrosol method is known as a technique for forming a metal carbide film more easily. This is a method in which diamond particles are immersed in a molten salt containing metal ions, and a carbide coating is formed on the particle surface by the reaction between metal ions and diamond. It has a feature that a coating with a substantially uniform thickness can be easily formed on the entire surface, and the coating can be formed on the surface of a submicron particle.
ダイヤモンド粒子を覆っている金属炭化物膜は、工具製作時の加熱状態で粒子を保持するマトリックス金属に濡れることによって、マトリックス内に強固に保持され、また加熱時の雰囲気ガスからダイヤモンドを保護する機能も発揮していると理解されている。 The metal carbide film covering the diamond particles is firmly held in the matrix by being wetted by the matrix metal that holds the particles in the heated state during tool fabrication, and also has the function of protecting the diamond from the atmospheric gas during heating. It is understood that it is performing.
別の分野の工具として、樹脂系の結合剤を用いる場合には、破砕されやすい粒子の脱落防止や、粒子の保持面積の向上を目的とし、全体として粒子の有効利用率を高める手段としてニッケルや銅の金属被覆を施した粒子が用いられている。
銅被覆を施した粒子においては、研磨加工の作用点に生じた熱を速やかに拡散させ、局部加熱による結合剤の劣化の防止が可能であることから、冷却剤を用いない研削・研磨加工用の粒子として広く用いられている。ただし使用に耐える銅めっきを直接ダイヤモンド粒子上に施すことは困難なため、固着強度の向上を目的とする中間層として、ダイヤモンド粒子表面にダイヤモンドの質量に対して20％程度のニッケルめっき層を施してから、銅めっき層を形成することが多い。 For particles coated with copper, it is possible to quickly diffuse the heat generated at the working point of polishing and prevent deterioration of the binder due to local heating. It is widely used as a particle. However, since it is difficult to apply copper plating that can withstand use directly onto diamond particles, a nickel plating layer of approximately 20% of the diamond mass is applied to the diamond particle surface as an intermediate layer for the purpose of improving the bond strength. After that, a copper plating layer is often formed.
これらの粒子においてはダイヤモンドと金属被覆との間の結合はあまり期待できず、粒子は単に金属被覆の殻の中に保持されている状態であるとも言える。このため金属被覆による粒子の保持効果は必ずしも十分ではなかった。 In these particles, the bond between the diamond and the metal coating cannot be expected so much, and it can be said that the particles are simply held in the shell of the metal coating. For this reason, the retention effect of the particle | grains by metal coating was not necessarily enough.
本発明の主な目的は前記した欠点の克服、特に、工具マトリックス中に保持使用された構成における熱放散性の良好なダイヤモンド研磨材粒子を提供することにある。 The main object of the present invention is to overcome the above-mentioned drawbacks, and in particular to provide diamond particles with good heat dissipation in a construction that is held and used in a tool matrix.
このような粒子は、本発明によれば、ダイヤモンド(炭素)に比して工具マトリックス(結合剤)への濡れ性の良好な金属炭化物膜を粒子のダイヤモンド表面に形成し、さらにその上に熱伝導性の良好な金属単体、或いはかかる金属を主体とする合金のめっきを施すことによって達成される。 According to the present invention, such a particle forms a metal carbide film on the diamond surface of the particle, which has better wettability to the tool matrix (binder) than diamond (carbon), and further heats the film. This is achieved by plating a single metal having good conductivity or an alloy mainly composed of such a metal.
本発明のダイヤモンド粒子は、従って、基体を構成するダイヤモンド粒子が表面に隣接する第一被覆層及び該被覆層の外面に隣接する第二被覆層を有し、上記第一被覆層はダイヤモンド粒子の表面において炭素と化学結合した、Ｔi、Ｚr、Ｈf、Ｖ、Ｎb、Ｔa、Ｃr、Ｍo、Ｗ、およびＳiから選ばれる第一の金属の炭化物を含有し、また上記第二被覆層は銅、銀又は金から選ばれる第二の金属単体、或いはこれら第二の金属を主体とする合金からなることを特徴とする。 Accordingly, the diamond particles of the present invention have a first coating layer in which the diamond particles constituting the substrate are adjacent to the surface and a second coating layer that is adjacent to the outer surface of the coating layer. Containing a carbide of a first metal selected from Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, and Si chemically bonded to carbon on the surface, and the second coating layer is made of copper, It consists of the 2nd metal simple substance chosen from silver or gold | metal | money, or the alloy which has these 2nd metals as a main component.
本発明によって作成されたダイヤモンド粒子は、内側に金属炭化物の薄層と、外側に高熱伝導性金属の被覆層とを有することから、工具マトリックス中に使用された際の良好な保持力及び熱放散性に基づく研削性能の向上に加えて、後述するように、外側被覆層を構成する第二の金属の高導電性に基づいて、電着工具作成時に高効率で電着操作を行えるという利点も得られる。 The diamond particles made according to the present invention have a thin layer of metal carbide on the inside and a coating layer of high thermal conductivity metal on the outside, so that they have good holding power and heat dissipation when used in a tool matrix. In addition to the improvement of grinding performance based on the properties, as described later, based on the high conductivity of the second metal constituting the outer coating layer, there is also an advantage that the electrodeposition operation can be performed with high efficiency at the time of electrodeposition tool creation. can get.
研削・研磨工具用ダイヤモンド粒子において、樹脂系結合剤用の粒子として上述したように銅めっきダイヤモンド粒子が多用されるが、かかる銅被覆粒子の製作に際しては、上述したように銅被覆層のダイヤモンド粒子に対する固着強度を高める目的から、ダイヤモンド粒子表面に予め下地層としてニッケルめっきを施すことが行われている。しかもこのニッケルめっきダイヤモンド粒子の全面を覆う必要があることから、10％(質量基準。以下同様)を超える厚めっきを必要とし、銅による熱拡散効果が十分に発揮されない欠点があった。 In diamond particles for grinding / polishing tools, copper-plated diamond particles are frequently used as resin-based binder particles as described above. When manufacturing such copper-coated particles, as described above, diamond particles in the copper-coated layer are used. For the purpose of increasing the adhesion strength to diamond, nickel plating is performed on the diamond particle surface in advance as an underlayer. In addition, since it is necessary to cover the entire surface of the nickel-plated diamond particles, thick plating exceeding 10% (mass basis; the same applies hereinafter) is required, and there is a drawback that the thermal diffusion effect by copper is not sufficiently exhibited.
例えば市販の銅被覆粒子では、下地層として粒子に対して約20％のニッケルめっきを施し、その上に約30％の銅めっきが施されている。この場合のめっき厚さは、粒子を直径100μmの真球と仮定すると、厚さ約2μmのニッケル層上に約4μmの銅被覆が存在する計算になる。 For example, in commercially available copper-coated particles, about 20% nickel plating is applied to the particles as an underlayer, and about 30% copper plating is applied thereon. The plating thickness in this case is calculated with a copper coating of about 4 μm on a nickel layer of about 2 μm thickness, assuming that the particles are true spheres with a diameter of 100 μm.
これに対し本発明においては、金属炭化物膜がダイヤモンド粒子表面に形成されることにより、上記のニッケルめっきによる中間層の形成が不要となる。しかも本発明方法によるパイロゾル法による炭化物形成では、nmオーダーの厚さの緻密な組織の薄膜を粒子全面に均一に形成することが可能であることから、中間層による熱拡散効果が向上し、結果として銅等第二の金属のめっき層による熱の拡散効果の向上によって樹脂系結合剤の劣化が抑制され、ダイヤモンドの脱落に起因する工具寿命の低下の阻止が可能となった。 On the other hand, in the present invention, since the metal carbide film is formed on the surface of the diamond particles, it is not necessary to form the intermediate layer by the nickel plating. Moreover, in the formation of carbide by the pyrosol method according to the present invention, it is possible to uniformly form a thin film of a dense structure with a thickness of the order of nm over the entire surface of the particle, so that the thermal diffusion effect by the intermediate layer is improved, resulting in As a result, the improvement of the heat diffusion effect by the plating layer of the second metal such as copper suppresses the deterioration of the resin binder, and it is possible to prevent the tool life from being reduced due to the falling off of the diamond.
例えば上記粒子の場合、0.5％のチタン添加によって粒子全面を覆うＴiＣ膜の形成が可能であるが、計算による膜の厚さは0.06μmに過ぎず、研削加工の際にダイヤモンド粒子先端部に生じた熱を被覆の銅へ散らす効果が、従来のニッケル下地層に比して格段に向上する。 For example, in the case of the above particles, it is possible to form a TiC film that covers the entire surface of the particle by adding 0.5% of titanium, but the calculated film thickness is only 0.06 μm and occurs at the tip of the diamond particle during grinding. The effect of dissipating heat to the coated copper is significantly improved compared to conventional nickel underlayers.
本発明において、外側被覆層の構成に用いられる銅、銀、金はまた、工具製作に用いられるほぼ全ての金属系マトリックス材料と相溶性を有する。このため、本発明の研磨材粒子は焼結工程を経由する工具製作用の粒子としても有用であって、マトリックス材料による粒子の保持強度の向上に伴う粒子の脱落防止、粒子の有効利用による工具寿命の向上、また切込量を大きくする高負荷加工が可能になると共に、工具の加工面における粒子の突き出し高さを大きく取れることによる、加工エネルギーの減少が可能となる。 In the present invention, copper, silver, and gold used in the construction of the outer coating layer are also compatible with almost all metal matrix materials used in tool fabrication. For this reason, the abrasive particles of the present invention are also useful as tool-making particles that pass through the sintering process, and prevent the particles from falling off due to the improvement of the retention strength of the particles by the matrix material. It is possible to improve the service life and perform high-load machining that increases the depth of cut, and to reduce machining energy by increasing the protruding height of particles on the machined surface of the tool.
また前記したニッケル下地めっきの代わりに金属炭化物被覆を施すことによる効果として、ダイヤモンド工具を用いた加工工程で生じる高温において、ダイヤモンドの黒鉛化、酸化を効果的に阻止する作用も挙げられる。ニッケルは高温において炭素の相転移を促進する作用があり、高圧力下では黒鉛からダイヤモンドへの反応を促進するが、常圧下では逆にダイヤモンドの黒鉛化を促進することが知られている。従ってダイヤモンドに接する被覆層材料としてニッケルに代えて金属炭化物を用いることで、黒鉛化促進の要因が除かれ、また緻密な金属炭化物被覆は、ダイヤモンドが酸素によって侵食されるのを効果的に阻止している。 Further, as an effect obtained by applying a metal carbide coating instead of the above-described nickel base plating, there is an effect of effectively preventing diamond graphitization and oxidation at a high temperature generated in a processing step using a diamond tool. Nickel has the effect of promoting the phase transition of carbon at high temperature, and promotes the reaction from graphite to diamond under high pressure, but conversely promotes the graphitization of diamond under normal pressure. Therefore, the use of metal carbide instead of nickel as the coating layer material in contact with diamond eliminates the factors that promote graphitization, and the dense metal carbide coating effectively prevents diamond from being eroded by oxygen. ing.
本発明品の別の用途として、細かなダイヤモンド粒子を用いた懸濁めっきにおいて、高導電性の第二被覆層をプラスに帯電させることにより、効率よく陰極側の支持体金属上に固着させることが可能となる。この手法を用いることにより、分散粒子濃度の低い条件における電着操作を用いて粒子が均一に分散した工具の製作、あるいは電着速度を高めることによる生産性の向上が可能となった。 As another application of the product of the present invention, in suspension plating using fine diamond particles, the highly conductive second coating layer is positively charged to be efficiently fixed on the support metal on the cathode side. Is possible. By using this method, it is possible to produce a tool in which particles are uniformly dispersed by using an electrodeposition operation under a condition where the concentration of dispersed particles is low, or to improve productivity by increasing the electrodeposition rate.
本発明において、ダイヤモンド粒子表面に隣接して形成される前記第一被覆層の量は、基体のダイヤモンドに対する質量比において0.5％以上で顕著である。ただし10％を超えると熱伝導阻害の原因となるので、これらの範囲内に設定するのが好適である。なお本発明における％表示は、別段の表示がない限り、全て質量基準による。 In the present invention, the amount of the first coating layer formed adjacent to the surface of the diamond particles is significant at a mass ratio of 0.5% or more to the diamond relative to the base. However, if it exceeds 10%, heat conduction is inhibited, so it is preferable to set within these ranges. In addition, unless otherwise indicated, the% display in this invention is based on a mass reference | standard.
一方、第二被覆層による効果は銅についてはダイヤモンドに対する比率が2％以上で顕著であるが、100％を超えるとダイヤモンド粒子本来の切れ味が得にくくなる。 On the other hand, the effect of the second coating layer is remarkable when the ratio of copper to diamond is 2% or more, but when it exceeds 100%, it becomes difficult to obtain the original sharpness of diamond particles.
本発明で使用するダイヤモンド粒子としては、平均粒径において0.5μm以上0.5mm以下のものが利用可能である。 As the diamond particles used in the present invention, those having an average particle diameter of 0.5 μm or more and 0.5 mm or less can be used.
本発明において前記第二の被覆層を構成する金属は必ずしも単体金属に限定されないが、熱や電気の伝導性の観点からは純度の高いほど好ましい。銅被覆については化学めっきによるのが簡便であるが、合金化に伴う熱伝導性低下の欠点があるので、電気めっき、あるいは蒸着などの方法がより好ましい。 In the present invention, the metal constituting the second coating layer is not necessarily limited to a single metal, but the higher the purity, the better from the viewpoint of heat and electrical conductivity. Although it is easy to use chemical plating for copper coating, there is a disadvantage of a decrease in thermal conductivity associated with alloying, so electroplating or vapor deposition is more preferable.
平均粒径100μmのダイヤモンド粉末ＩＲＶ140/170メッシュ(トーメイダイヤ製) 100ｇと、0.5ｇのチタン粉末(粒径40μm)とを容量500mlのステンレスビーカーへ入れ、モル比でＮaＣl:ＫＣl=1:1の混合塩(共晶温度約660℃)約300ｇを加えた。このビーカーを炉内で800℃に加熱し2時間保持した。 100 g of diamond powder with an average particle size of 100 μm IRV140 / 170 mesh (made by Tomei Diamond) and 0.5 g of titanium powder (particle size of 40 μm) are put into a stainless steel beaker with a capacity of 500 ml, and a molar ratio of NaCl: KCl = 1: 1. About 300 g of mixed salt (eutectic temperature of about 660 ° C.) was added. The beaker was heated to 800 ° C. in a furnace and held for 2 hours.
放冷後、炉より取り出し、ビーカー中の塩を水に溶かして除去し、次いで6N-ＨＣlを加えて1時間煮沸し、未反応チタンを溶解・除去した。さらに水洗・乾燥工程を経て、約0.5％のＴiＣで被覆された粒子を得た。得られた粉末は黒色を呈しており、Ｘ線回折によって、ダイヤモンドと共にＴiＣと同定された。また計算上のＴiＣによる被覆厚さは約0.06μmと見積もられた。 After standing to cool, it was taken out from the furnace, the salt in the beaker was dissolved in water and removed, then 6N-HCl was added and boiled for 1 hour to dissolve and remove unreacted titanium. Further, after being washed with water and dried, particles coated with about 0.5% TiC were obtained. The obtained powder had a black color and was identified as TiC together with diamond by X-ray diffraction. The calculated coating thickness by TiC was estimated to be about 0.06 μm.
次いで無電解銅めっきによって、ダイヤモンド粒子に対して30％の銅被覆をＴiＣ上に形成した。めっき浴の組成はg/ｌ表示で、硫酸銅:10、ロッシェル塩:50、水酸化ナトリウム:10、ホルマリン:10ml/lとした。 A 30% copper coating on the diamond particles was then formed on the TiC by electroless copper plating. The composition of the plating bath was expressed in g / l, copper sulfate: 10, Rochelle salt: 50, sodium hydroxide: 10, formalin: 10 ml / l.
得られた銅被覆の厚さは計算値で約3μmと見積もられた。この粒子を用いて下記条件によるレジンボンド砥石を作製、ダイヤモンド焼結体表面の乾式平坦化加工に使用し、性能を従来技術による銅被覆粒子を用いた砥石と比較した。
砥石の形式 6A2 ディスク型砥石 外径 225mm、内径 125mm
結合剤 エポキシ樹脂
集中度 100
砥石回転数 1500 rpm
押付け圧力 50kgf/cm2
The thickness of the obtained copper coating was estimated to be about 3 μm by calculation. Using these particles, a resin bond grindstone was produced under the following conditions, used for dry flattening of the surface of the diamond sintered body, and the performance was compared with a grindstone using copper-coated particles according to the prior art.
Grinding wheel type 6A2 Disc type grinding wheel OD 225mm, ID 125mm
Binder Epoxy resin Concentration 100
Grinding wheel speed 1500 rpm
Pressing pressure 50kgf / cm 2
対比の結果、従来技術による砥石の寿命が平均１ケ月であったのに対し、本発明による粒子を用いた砥石寿命は平均1.6ケ月であり、顕著な粒子の脱落阻止効果が認められた。 As a result of comparison, while the life of the grindstone according to the prior art averaged 1 month, the life of the grindstone using the particles according to the present invention averaged 1.6 months, and a remarkable drop-off prevention effect was recognized.
平均粒径21μmのダイヤモンド粉末ＩＲＭ20-30 (トーメイダイヤ製) 200ｇと、4.5ｇのチタン粉末(粒径40μm)とを用い、実施例１と同じ方法でダイヤモンド表面へ約0.04μm(計算値)のＴiＣ被覆を形成した。得られたＴiＣ被覆ダイヤモンドの半量にはさらに、ワット浴を用いて銅めっきを行い、約１μm(計算値)の銅めっき層を形成した。 Using diamond powder IRM20-30 (made by Tomei Diamond) with an average particle size of 21 μm and 4.5 g of titanium powder (particle size of 40 μm), approximately 0.04 μm (calculated value) was applied to the diamond surface in the same manner as in Example 1. A TiC coating was formed. Half of the obtained TiC-coated diamond was further subjected to copper plating using a Watt bath to form a copper plating layer of about 1 μm (calculated value).
ＴiＣ被覆のままの粒子と、さらにその上に銅めっきで被覆した粒子とを用い、それぞれスルファミン酸ニッケル浴中に懸濁させて、ニッケルめっき条件における浴抵抗値の測定を行った。めっき液中における懸濁量はそれぞれ30g/lとし、陽極としてはニッケル板を、陰極には水酸化ナトリウム水溶液中で脱脂し次いで希塩酸中で洗浄した1.2mmφSUS線を用いた。 The particles as they were coated with TiC and the particles coated with copper plating thereon were suspended in a nickel sulfamate bath, and the bath resistance value was measured under nickel plating conditions. The amount of suspension in the plating solution was 30 g / l, a nickel plate was used as the anode, and a 1.2 mmφ SUS wire that was degreased in an aqueous sodium hydroxide solution and then washed in dilute hydrochloric acid was used as the cathode.
粒子を懸濁させた液の抵抗値測定の結果、ＴiＣ被覆のままの粒子が約60Ω/cmであったのに対し、上に銅めっきを施した粒子では約40Ω/cmであり、懸濁めっきに好ましい効果が得られることが分かった。 As a result of measuring the resistance value of the liquid in which the particles were suspended, the particles with the TiC coating were about 60 Ω / cm, whereas the particles plated with copper were about 40 Ω / cm. It was found that a favorable effect can be obtained for plating.
本発明のダイヤモンド粒子は、研磨材粒子をレジンで結合した工具としての使用において、或いは電着工具の製作において、格段の性能及び操作性が達成される。
The diamond particles of the present invention achieve remarkable performance and operability when used as a tool in which abrasive particles are bonded with a resin, or in the production of an electrodeposition tool.
Claims (5)
(2) 次いで前記第一被覆層の上に電気めっきまたは化学めっきによりＣu、Ａg及びＡuから選ばれる第二の金属単体又は該第二の金属を主体とする合金からなる第二の被覆層を形成する段階
を有する二重被覆ダイヤモンド研磨材粒子の製造方法。
(1) Disperse a diamond powder sized in molten salt and a powder of a first metal selected from Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, and Si, Forming a first coating layer comprising a carbide of the metal on the surface of the particles;
(2) Next, on the first coating layer, a second coating layer made of a second metal simple substance selected from Cu, Ag and Au or an alloy mainly composed of the second metal by electroplating or chemical plating. A method for producing double-coated diamond abrasive particles comprising the step of forming.
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| JP2015178425A (en) * | 2014-03-19 | 2015-10-08 | 国立大学法人福井大学 | Diamond composite particle and production method thereof |
| CN108747874A (en) * | 2018-05-31 | 2018-11-06 | 芜湖昌菱金刚石工具有限公司 | A kind of scuff-resistant coating diamond composite and preparation method thereof |
| CN109159037A (en) * | 2018-09-20 | 2019-01-08 | 王建东 | A kind of preparation method of honing stone |
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| CN109159037B (en) * | 2018-09-20 | 2020-10-23 | 施仙增 | Preparation method of honing oilstone |
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