JP4589154B2 - Seal ring - Google Patents

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JP4589154B2
JP4589154B2 JP2005065790A JP2005065790A JP4589154B2 JP 4589154 B2 JP4589154 B2 JP 4589154B2 JP 2005065790 A JP2005065790 A JP 2005065790A JP 2005065790 A JP2005065790 A JP 2005065790A JP 4589154 B2 JP4589154 B2 JP 4589154B2
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seal ring
plate
calcium carbonate
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resistance
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JP2006249187A (en
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美香 斉藤
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Riken Corp
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本発明は、自動車のオートマチックトランスミッション(Automatic Transmission, 以下「AT」という。)のシールリングに関し、特に、金型鋳造したアルミニウム合金(以下「アルミ合金」という。)製回転軸に摺接し、オートマチックトランスミッション油(Automatic Transmission Fluid, 以下「ATF」という。)をシールする回転軸シールリングに関する。   The present invention relates to a seal ring for an automatic transmission (hereinafter referred to as “AT”) of an automobile, and more particularly to an automatic transmission that is in sliding contact with a rotating shaft made of a die-cast aluminum alloy (hereinafter referred to as “aluminum alloy”). The present invention relates to a rotary shaft seal ring that seals oil (Automatic Transmission Fluid, hereinafter referred to as “ATF”).

自動車の燃費向上を目的に、自動車部品の小型化、薄肉化、あるいはアルミニウム等の軽金属の利用等、様々な試みが行われている。ATにおいても、回転軸及びハウジングにアルミ合金を用いる場合が多くなってきており、燃費の良い無段変速機(Continuously Variable Transmission)は従来の上位大型車だけでなく一般小型車にも実車搭載されるようになり、市場ではアルミ合金等の軟質系軽金属に対応可能な小径シールリングが求められている。従来の鉄系材料の回転軸やハウジングでは、シールリング材料としては鋳鉄又は特にポリテトラフルオロエチレン(Polytetrafluoroethylene, 以下「PTFE」という。)が便利に用いられてきた。特に、PTFEは優れた性能を発揮してきた。しかし、そのPTFEもアルミ合金製回転軸に対しては、高温且つ高速摺動条件下で相手攻撃性が強くなり、PTFEのシールリングもアルミ合金製回転軸も共に異常摩耗を引き起こすという問題を経験した。PTFEが相手金属と摺動するときの摩擦のメカニズムは、最初に摩耗したPTFEが相手金属面に移行してPTFE同士の摺動となって、摩擦係数が下がると共に摩耗量も減少すると言われている。相手金属が鉄系材料の場合はPTFEの相手金属面への移行定着がスムーズに行われるのに対し、相手金属が軟らかいアルミ合金の場合にはPTFEの移行定着が困難なため高速高面圧の摺動条件下ではアルミの凝着が起こり、上述のような異常摩耗を引き起こす。   For the purpose of improving the fuel efficiency of automobiles, various attempts have been made, such as miniaturization and thinning of automobile parts or the use of light metals such as aluminum. Even in ATs, aluminum alloys are often used for the rotating shaft and housing, and continuously variable transmission with good fuel efficiency can be mounted not only on conventional high-end large vehicles but also on general small vehicles. Accordingly, there is a demand for a small-diameter seal ring that can handle soft light metals such as aluminum alloys. Conventional rotary shafts and housings of iron-based materials have conveniently used cast iron or particularly polytetrafluoroethylene (hereinafter referred to as “PTFE”) as a seal ring material. In particular, PTFE has demonstrated excellent performance. However, the PTFE also has a problem that against the aluminum alloy rotating shaft, the opponent's aggression becomes stronger under high temperature and high speed sliding conditions, and both the PTFE seal ring and the aluminum alloy rotating shaft cause abnormal wear. did. The friction mechanism when PTFE slides against the mating metal is said to be that the PTFE that was first worn moves to the mating metal surface and slides between the PTFE, reducing the friction coefficient and reducing the amount of wear. Yes. When the mating metal is an iron-based material, PTFE can be transferred and fixed smoothly to the mating metal surface. Under sliding conditions, aluminum adhesion occurs, causing abnormal wear as described above.

このようなアルミ合金製回転軸に対するPTFEの問題点に対し、PTFEに代わって高温エンジニアリングポリマーとして代表的なポリエーテルエーテルケトン樹脂(Polyetheretherketon, 以下「PEEK」という。)を用いることによって対応が取られている。PEEKは、PTFEと比較して、引張強度、硬度が約4倍あるが引張伸びが1/10以下であり柔軟性に欠けるものの、アルミの凝着が起こりにくいという性質を持つ。アルミ合金に対し同様の性質を持つ樹脂として、ポリエーテルケトン(Polyetherketon, 以下「PEK」という。)、ポリエーテルニトリル(Polyethernitryl、以下「PEN」という。)、ポリフェニレンファルファイド(Polyphenylenesulfide, 以下「PPS」という。)があげられる。   The PTFE problem for aluminum alloy rotating shafts can be addressed by using a typical polyetheretherketone resin (hereinafter referred to as “PEEK”) as a high temperature engineering polymer instead of PTFE. ing. PEEK has about four times the tensile strength and hardness compared to PTFE, but has a tensile elongation of 1/10 or less and lacks flexibility, but has the property that aluminum does not easily adhere. As resins having similar properties to aluminum alloys, polyetherketon (hereinafter referred to as “PEK”), polyethernitrile (hereinafter referred to as “PEN”), polyphenylenesulfide (hereinafter referred to as “PPS”). Said).

一般に、PTFEやPEEK単体では、AT用シールリングとしての要求性能を満足しないので耐摩耗性、弾性率、耐クリープ性、耐熱性、耐圧性、熱伝導性、耐油性、潤滑性、成形性等の要求性能を満足させるために複合化して用いられるのが一般的である。具体的には、機械的特性や耐摩耗性を向上させるためには、ガラス繊維、炭素繊維、チタン酸カリウムウイスカー等の繊維状充填材又は黒鉛、マイカ、タルク等の鱗片状充填材が添加され、低摩擦特性を付与するためにPTFE、黒鉛、二硫化モリブデン等の固体潤滑材が添加されている。PEEK材料に関していえば、PEEKに炭素繊維、PTFE、タルク又は炭酸カルシウムを複合するもの(特開平5-262976号:特許文献1)、PEEKに炭素繊維、PTFE、モース硬度3以下の粒状又はウイスカー状の硫酸マグネシウム又は硫酸カルシウムを複合するもの(特開2001-49111号:特許文献2)等が提案されている。   In general, PTFE and PEEK alone do not satisfy the required performance as a seal ring for AT, so wear resistance, elastic modulus, creep resistance, heat resistance, pressure resistance, thermal conductivity, oil resistance, lubricity, moldability, etc. In order to satisfy the required performance, it is generally used in combination. Specifically, in order to improve mechanical properties and wear resistance, fibrous fillers such as glass fibers, carbon fibers, and potassium titanate whiskers, or scaly fillers such as graphite, mica, and talc are added. In order to impart low friction properties, solid lubricants such as PTFE, graphite and molybdenum disulfide are added. Regarding PEEK materials, carbon fiber, PTFE, talc, or calcium carbonate is combined with PEEK (Japanese Patent Laid-Open No. 5-262976: Patent Document 1), carbon fiber, PTFE, granular or whisker shape with Mohs hardness of 3 or less A combination of magnesium sulfate or calcium sulfate (Japanese Patent Laid-Open No. 2001-49111: Patent Document 2) has been proposed.

また、PEEKは極めて高価であり、コスト面で市場が満足して受け入れる状況に至っていないのも実情であって、使用するPEEKをできるだけ少なくして要求性能を満足させることも求められている。しかし、充填材を多量に配合することで脆性が増すので、シールリングにおいては合口部を拡げて軸に取り付ける際に、特に外径寸法が30mm以下の小型のシールリングにおいては、合口部が許容弾性変形量を超えて折損しやすくなる等の問題が生じる。   In addition, PEEK is extremely expensive, and it is a fact that the market has not yet reached a satisfactory situation in terms of cost, and there is a demand for satisfying the required performance by using as few PEEK as possible. However, since the brittleness increases by adding a large amount of filler, when the seal ring is expanded and attached to the shaft, the joint is allowed, especially for small seal rings with an outer diameter of 30 mm or less. Problems such as breakage exceeding the amount of elastic deformation occur.

脆性を改善する方法として、PPS樹脂にエラストマーを配合することで柔軟性が付与されることは知られている(特開平5-239350号:特許文献3)。しかし、PEEKのような高温で成形する樹脂に耐熱性の低いエラストマーを添加すると、耐熱性の低下や成形時のガス発生等の問題がある。   As a method for improving brittleness, it is known that flexibility is imparted by blending an elastomer with a PPS resin (Japanese Patent Laid-Open No. 5-239350: Patent Document 3). However, when an elastomer having low heat resistance is added to a resin molded at a high temperature such as PEEK, there are problems such as a decrease in heat resistance and gas generation during molding.

また、耐衝撃性を改善するといわれている炭酸カルシウムと、弾性率を改善するといわれているタルク、マイカ、クレー等の板状フィラーとを高速撹拌によって均一に混合粉砕した凝集塊の無い複合フィラーが知られている(特開2002-80631号:特許文献4)。しかし、複合される合成樹脂としてはホモポリプロピレンやブロックポリプロピレンのポリオレフィン系樹脂、ナイロン6のポリアミド系樹脂、PETのポリエステル系樹脂であって、AT用シールリングを想定したPEEKをベースに炭酸カルシウムと板状フィラーの含有率を最適化していないため、耐折損性(脆性)は改善されても耐摩耗性が不十分な場合があり、これらの複合フィラーをAT用シールリングに適用しても、必ずしも耐折損性と耐摩耗性とのバランスがとれていない場合があった。   In addition, there is a composite filler without agglomerates obtained by uniformly mixing and grinding calcium carbonate, which is said to improve impact resistance, and plate-like fillers, such as talc, mica and clay, which are said to improve elastic modulus, by high-speed stirring. Known (Japanese Patent Laid-Open No. 2002-80631: Patent Document 4). However, synthetic resins to be compounded include homopolypropylene and block polypropylene polyolefin resins, nylon 6 polyamide resins, and PET polyester resins, which are based on PEEK assuming an AT seal ring and calcium carbonate and plate However, even if the fracture resistance (brittleness) is improved, the wear resistance may be insufficient even if the fracture resistance (brittleness) is improved. In some cases, the breakage resistance and the wear resistance were not balanced.

特開平5-262976号公報Japanese Patent Laid-Open No. 5-262976 特開2001-49111号公報Japanese Patent Laid-Open No. 2001-49111 特開平5-239350号公報Japanese Patent Laid-Open No. H5-239350 特開2002-80631号公報JP 2002-80631 A

従って、本発明の目的は、アルミ合金と摺接するAT用シールリングにおいて、特に外径寸法が30mm以下の小型のシールリングにおいて効果のあることを期待しているが、PEEKを65重量%以下に減じても、優れた耐摩耗性及び低相手攻撃性を有し、合口部を拡げて軸に取り付ける際に合口部が許容弾性変形量を超えて折損することのないAT用シールリングを提供することである。   Therefore, the object of the present invention is expected to be effective in the AT seal ring that is in sliding contact with the aluminum alloy, particularly in a small seal ring having an outer diameter of 30 mm or less. However, PEEK is reduced to 65 wt% or less. Providing an AT seal ring that has excellent wear resistance and low opponent attack even if it is reduced and does not break beyond the allowable elastic deformation when the joint is expanded and attached to the shaft. That is.

上記目的に鑑み鋭意研究の結果、本発明者は、PEEK材料への充填材として特定サイズの炭素繊維の他、主要な充填材として炭酸カルシウムとタルクを選択し、その充填粉末のサイズと量を最適化することにより、優れた耐摩耗性と低相手攻撃性に加え、耐折損性の著しく改善されたAT用シールリングが得られることを見いだし、本発明に想到した。   As a result of diligent research in view of the above object, the present inventor selected calcium carbonate and talc as main fillers in addition to carbon fibers of a specific size as fillers for PEEK materials, and determined the size and amount of the filled powder. As a result of the optimization, it was found that an AT seal ring with significantly improved breakage resistance in addition to excellent wear resistance and low opponent attack properties was obtained, and the present invention was conceived.

すなわち、本発明のシールリングは、PEEK 65重量%以下、平均繊維径3〜10μmの炭素繊維10〜30重量%、平均粒径0.5〜5μmの炭酸カルシウム粉末と平均板径0.1〜5μmの板状タルク粉末を合計10〜35重量%含有することを特徴とする。量的には、炭酸カルシウム粉末/板状タルク粉末の重量比率で0.2〜1.2の範囲内であることが好ましい。また、板状タルク粉末の一部を平均板径10μm以下の鱗片状黒鉛に替えても、特に耐摩耗性の観点で好適である。   That is, the seal ring of the present invention is PEEK 65% by weight or less, carbon fiber 10-30% by weight with an average fiber diameter 3-10 μm, calcium carbonate powder with an average particle size 0.5-5 μm and a plate shape with an average plate diameter 0.1-5 μm. It is characterized by containing 10 to 35% by weight of talc powder. Quantitatively, the weight ratio of calcium carbonate powder / plate-like talc powder is preferably in the range of 0.2 to 1.2. Further, even if a part of the plate-like talc powder is replaced with scaly graphite having an average plate diameter of 10 μm or less, it is particularly preferable from the viewpoint of wear resistance.

炭酸カルシウム粉末は微細になると凝集塊を形成する傾向が強いので、凝集塊を粉砕するため、炭酸カルシウム粉末と板状タルク粉末を乾式で高速撹拌によって均一に混合粉砕することはなお好ましい。   Since the calcium carbonate powder has a strong tendency to form an agglomerate when it becomes finer, it is still preferable to uniformly grind the calcium carbonate powder and the plate-like talc powder by high-speed agitation in order to pulverize the agglomerate.

本発明のシールリングは、PEEK 65重量%以下、平均繊維径3〜10μmの炭素繊維10〜30重量%、平均粒径0.5〜5μmの炭酸カルシウム粉末と平均板径0.1〜5μmの板状タルク粉末を合計10〜35重量%含有するので、高価なPEEKの使用量を減じ、且つ、炭素繊維、及び板状タルク粉末の複合により優れた強度及び耐摩耗性に加え、均一に分散した炭酸カルシウム粉末により改善された耐折損性を有する。このため、本発明のシールリングは、例え、外径寸法が30mm以下の小型のシールリングにおいても、合口部を拡げて軸に取り付ける際に合口部が許容弾性変形量を超えて折損することがなく容易に軸に取り付けできるものになる。   The seal ring of the present invention comprises PEEK 65% by weight or less, carbon fiber 10-30% by weight with an average fiber diameter of 3-10 μm, calcium carbonate powder with an average particle diameter of 0.5-5 μm, and plate-like talc powder with an average plate diameter of 0.1-5 μm 10 to 35% by weight in total, so that the amount of expensive PEEK used is reduced, and in addition to excellent strength and wear resistance due to the composite of carbon fiber and plate-like talc powder, uniformly dispersed calcium carbonate powder Has improved breakage resistance. For this reason, the seal ring of the present invention may break even when the joint part is expanded and attached to the shaft even if it is a small seal ring having an outer diameter of 30 mm or less, and the joint part exceeds the allowable elastic deformation amount. And can be easily attached to the shaft.

本発明に用いるPEEK並びにその一部又は全部を置き換えることのできるPEK、PEN及びPPSは、高い耐熱性に加え、優れた機械的性質、電気的性質、耐薬品性を有するものであるが、それぞれ市販されている周知の樹脂を使用することができる。いずれも高価な樹脂であるが、それらを65重量%以下に抑えることでコスト面での市場の要求に近づけることが可能となる。   PEEK used in the present invention and PEK, PEN and PPS which can replace part or all of them have excellent mechanical properties, electrical properties and chemical resistance in addition to high heat resistance. A well-known resin marketed can be used. Although both are expensive resins, it is possible to approach the market demand in terms of cost by limiting them to 65% by weight or less.

次に、本発明に用いる炭素繊維は、平均繊維径3〜10μmとする。一般に炭素繊維は平均繊維径1〜30μm、平均長さ数10μm〜数mmのものが市販されているが、特にポリアクリロニトリル(PAN)系炭素繊維で平均繊維径3〜10μmのものが好ましい。平均繊維径が3μm未満では繊維同士の絡みにより均一分散が困難であり、混練時に繊維が折れて短繊維となり、また10μmを越えるものでは逆に繊維強度も比較的低くなるので繊維強化による機械的性質の向上が十分望めない。このような炭素繊維の配合割合は10〜30重量%とする。10重量%未満では繊維強化による機械的性質の向上が十分でなく、また30重量%を越えると複合樹脂の溶融流動性を著しく低下させシールリングの射出成形が困難となる。   Next, the carbon fiber used in the present invention has an average fiber diameter of 3 to 10 μm. In general, carbon fibers having an average fiber diameter of 1 to 30 μm and an average length of several tens of μm to several mm are commercially available. In particular, polyacrylonitrile (PAN) carbon fibers having an average fiber diameter of 3 to 10 μm are preferable. If the average fiber diameter is less than 3μm, uniform dispersion is difficult due to the entanglement of the fibers, and when kneading, the fiber breaks to become short fibers, and if it exceeds 10μm, the fiber strength is relatively low, so mechanical strength by fiber reinforcement The improvement in properties cannot be expected sufficiently. The blending ratio of such carbon fibers is 10 to 30% by weight. If it is less than 10% by weight, the mechanical properties are not sufficiently improved by fiber reinforcement, and if it exceeds 30% by weight, the melt flowability of the composite resin is remarkably lowered and it becomes difficult to injection-mold the seal ring.

次に、本発明に用いる充填材としての炭酸カルシウム粉末は平均粒径0.5〜5μmとする。この範囲の平均粒径において、炭酸カルシウム粉末の均一分散により耐折損性が改善される。平均粒径が1μm未満の炭酸カルシウム粉末を通常に混合しただけでは、粒子間の凝集が起こって均一分散が困難となり、また5μmを越えるものでも耐折損性の向上が十分でなくなる。但し、炭酸カルシウム粉末と同時に添加される板状タルク粉末と一緒に高速撹拌による混合粉砕を行った場合には、平均粒径0.5〜1μmにおいても凝集塊が粉砕され均一分散が可能となる。また、同時に添加される板状タルク粉末は、平均板径0.1〜5μmとする。板状タルクは、主として弾性率の向上による機械的性質の改善のほかに、耐熱性、摺動性及び寸法安定性の向上並びに射出成形時のヒケやそりの防止に効果がある。板状タルクも、炭酸カルシウム粉末と同様に、通常、平均粒径が1μm未満の粉末を混合しただけでは、粒子間の凝集が起こって均一分散が困難となる。また5μmを越えると耐折損性が著しく低下する。高速撹拌による混合粉砕を行った場合、板状タルクは炭酸カルシウムに比べ、より微細に粉砕され、平均粒径0.1〜1μmにおいても凝集塊が粉砕され均一分散が可能となる。   Next, the calcium carbonate powder as the filler used in the present invention has an average particle size of 0.5 to 5 μm. In the average particle diameter within this range, the breakage resistance is improved by the uniform dispersion of the calcium carbonate powder. If calcium carbonate powder having an average particle size of less than 1 μm is usually mixed, agglomeration between particles occurs and uniform dispersion becomes difficult, and if the particle size exceeds 5 μm, the breakage resistance is not sufficiently improved. However, when mixed and pulverized by high-speed stirring together with the plate-like talc powder added simultaneously with the calcium carbonate powder, the agglomerates are pulverized and uniformly dispersed even at an average particle size of 0.5 to 1 μm. Further, the plate-like talc powder added at the same time has an average plate diameter of 0.1 to 5 μm. The plate-like talc is effective in improving heat resistance, slidability and dimensional stability, and preventing sink marks and warpage during injection molding, in addition to improving mechanical properties mainly by improving elastic modulus. Similarly to the calcium carbonate powder, the plate-like talc is usually mixed only with a powder having an average particle diameter of less than 1 μm, and the particles are aggregated and uniform dispersion becomes difficult. On the other hand, if it exceeds 5 μm, the breakage resistance is significantly reduced. When mixed and pulverized by high-speed stirring, plate-like talc is pulverized more finely than calcium carbonate, and agglomerates are pulverized and evenly dispersed even with an average particle size of 0.1 to 1 μm.

これらの炭酸カルシウム粉末と板状タルク粉末の配合割合は、合計で10〜35重量%とする。10重量%未満では耐摩耗性が不足し、安価な充填材の量が少ないので高価なPEEK使用量の低減が十分でなく、また35重量%を越えると複合樹脂の溶融流動性を著しく低下させるとともに、炭酸カルシウム添加によりpHが上昇し、ベース樹脂がゲル化しやすくなるためシールリングの射出成形が困難となる。   The blending ratio of these calcium carbonate powder and plate-like talc powder is 10 to 35% by weight in total. If it is less than 10% by weight, the wear resistance is insufficient, and the amount of inexpensive filler is small, so that the amount of expensive PEEK used is not sufficiently reduced, and if it exceeds 35% by weight, the melt fluidity of the composite resin is significantly reduced. At the same time, the pH increases due to the addition of calcium carbonate, and the base resin is easily gelled, which makes injection molding of the seal ring difficult.

本発明のシールリングは、耐欠損性と耐摩耗性の両特性において優れている必要があり、いずれか一方のみが改善されただけでは十分ではない。耐欠損性と耐摩耗性のバランスという観点で、複合する炭酸カルシウム粉末の配合割合と板状タルク粉末の配合割合の比率は重要である。本発明では、炭酸カルシウム粉末重量/板状タルク粉末重量比率が0.2〜1.2の範囲とする。重量比率0.2未満では炭酸カルシウムによる耐欠損性の改善が十分でなく、また重量比率1.2を越えると耐摩耗性が不十分となるとともに、炭酸カルシウムによるpH値の上昇が起こる。好ましくは0.3〜1.1の範囲とする。   The seal ring of the present invention needs to be excellent in both fracture resistance and wear resistance, and it is not sufficient that only one of them is improved. From the viewpoint of a balance between fracture resistance and wear resistance, the ratio of the compounding ratio of the calcium carbonate powder and the compounding ratio of the plate-like talc powder is important. In the present invention, the calcium carbonate powder weight / plate-like talc powder weight ratio is in the range of 0.2 to 1.2. If the weight ratio is less than 0.2, the defect resistance due to calcium carbonate is not sufficiently improved, and if the weight ratio exceeds 1.2, the wear resistance becomes insufficient and the pH value increases due to calcium carbonate. Preferably it is set as the range of 0.3-1.1.

さらに、本発明のシールリングにおいては、摺動特性を向上させ耐摩耗性をさらに改善させるため、板状タルク粉末の一部を平均板径10μm以下の鱗片状黒鉛に置き換えることができる。但し、鱗片状黒鉛の平均板径が10μmを越えるとシールリングの耐折損性を低下させる。また板状タルク粉末に置き換える鱗片状黒鉛の配合割合は7重量%未満が好ましい。   Furthermore, in the seal ring of the present invention, a part of the plate-like talc powder can be replaced with scaly graphite having an average plate diameter of 10 μm or less in order to improve the sliding characteristics and further improve the wear resistance. However, when the average plate diameter of the flake graphite exceeds 10 μm, the breakage resistance of the seal ring is lowered. Further, the blending ratio of the flake graphite replaced with the plate-like talc powder is preferably less than 7% by weight.

本発明を以下の実施例によりさらに詳細に説明するが、本発明はこれらの例に限定されるものではない。   The present invention will be described in more detail with reference to the following examples, but the present invention is not limited to these examples.

実施例1〜4(J1〜4)及び比較例1〜3(H1〜3)
粉末状PEEK、平均繊維径6.5μmの炭素繊維、平均粒径1.4μmの炭酸カルシウム及び平均板径3.2μmの板状タルクを表1に示した各配合割合で、まず、押出機において温度400℃、スクリュウ回転数50rpm、粉体供給回転数65rpmの条件で混合し、約3mm径で長さ3〜4mmのペレットを所定量作製した。次に、摩耗試験用に呼径(外径)60.0mm、幅2.0mm、厚さ2.0mmの特殊ステップ合口形状の摩耗試験用テストピース、及び、呼径(外径)24.5mm、幅1.8mm、厚さ1.4mmの折損試験用テストピースに、金型温度170℃、成形温度340〜420℃、射出速度30mm/sec、成形圧力130MPaの条件にて前記ペレットを用いて射出成形した。
Examples 1-4 (J1-4) and Comparative Examples 1-3 (H1-3)
Powdered PEEK, carbon fiber with an average fiber diameter of 6.5 μm, calcium carbonate with an average particle diameter of 1.4 μm, and plate-like talc with an average plate diameter of 3.2 μm are mixed in the proportions shown in Table 1 and first, the temperature is 400 ° C. in an extruder. The mixture was mixed under the conditions of a screw rotation speed of 50 rpm and a powder supply rotation speed of 65 rpm to produce a predetermined amount of pellets having a diameter of about 3 mm and a length of 3 to 4 mm. Next, a wear test test piece with a special step joint shape with a nominal diameter (outer diameter) of 60.0 mm, a width of 2.0 mm, and a thickness of 2.0 mm, and a nominal diameter (outer diameter) of 24.5 mm and a width of 1.8 mm. A test piece for breakage test having a thickness of 1.4 mm was injection molded using the pellets under conditions of a mold temperature of 170 ° C., a molding temperature of 340 to 420 ° C., an injection speed of 30 mm / sec, and a molding pressure of 130 MPa.

摩耗試験は図1に模式的に示すスラスト型摩耗試験機を用いて行った。この試験機は、オイル中で、一定速度で回転するシールリングを固定するホルダと、それに対向し一定面圧で加圧するアルミ円板を固定するホルダから構成され、評価は所定の摩擦距離を運転した後のシールリングの摩耗量とアルミ円板の摩耗量を測定することによって行うものである。摩耗試験の条件としては、摩擦速度6.7m/sec、接触面圧1MPa、相手材は表面粗さ(Rz)1μm のJIS2024のアルミ合金円板、摩擦距離44km、摩擦方式ATF油滑りで油温は成り行きとした。なお、シールリングテストピースの摺動面は実機の状況に近い状況とするため射出成形した面のままとした。   The abrasion test was conducted using a thrust type abrasion tester schematically shown in FIG. This testing machine consists of a holder that fixes a seal ring that rotates at a constant speed in oil, and a holder that fixes an aluminum disk that presses against it with a constant surface pressure. This is done by measuring the amount of wear of the seal ring and the amount of wear of the aluminum disc. The conditions of the wear test were as follows: friction speed 6.7m / sec, contact surface pressure 1MPa, mating material JIS2024 aluminum alloy disk with surface roughness (Rz) 1μm, friction distance 44km, friction method ATF oil sliding, It happened. In addition, the sliding surface of the seal ring test piece was left as the injection-molded surface in order to make the situation close to that of the actual machine.

また、折損試験は、図2に模式的に示す専用試験機を用いて行った。図2の円錐状の治具に沿ってシールリングを一定速度で押し広げてゆき、シールリングが折損する直前の最大内径を測定することによって耐折損性を評価するものである。本発明の目的とする耐折損性は、PEEK70重量%、炭素繊維20重量%、その他充填物10重量%からなる市販のシールリングの耐欠損性と同等の特性を有することとして、このシールリングの耐折損性を100として百分率表記した。   Further, the breakage test was conducted using a dedicated testing machine schematically shown in FIG. The seal ring is expanded at a constant speed along the conical jig shown in FIG. 2, and the fracture resistance is evaluated by measuring the maximum inner diameter immediately before the seal ring breaks. Fracture resistance targeted by the present invention is equivalent to that of a commercially available seal ring comprising 70% by weight of PEEK, 20% by weight of carbon fiber, and 10% by weight of other fillers. Expressed as a percentage, with break resistance as 100.

表1の実施例1〜4(J1〜4)、比較例1〜3(H1〜3)の摩耗試験結果及び折損試験結果を同表中に示した。本発明の範囲においては自己摩耗量が10μm以下で且つ耐折損性が100%以上であった。   The wear test results and breakage test results of Examples 1 to 4 (J1 to 4) and Comparative Examples 1 to 3 (H1 to 3) in Table 1 are shown in the same table. Within the scope of the present invention, the amount of self-wear was 10 μm or less, and the fracture resistance was 100% or more.

Figure 0004589154
Figure 0004589154

実施例5〜7(J5〜7)及び比較例4〜6(H4〜6)
実施例2(J2)と同じ配合割合の組成にて、炭酸カルシウム粉末及び板状タルク粉末の粒径又は板径を表2に示す組み合わせにして摩耗試験用テストピース及び折損試験用テストピースを実施例2(J2)と同じ方法で作製した。実施例5、6(J5, 6)及び比較例4(H4)は、実施例2(J2)の粉末サイズの原料を用いてヘンシェルミキサーで高速撹拌により撹拌条件を変えて混合粉砕したものである。摩耗試験及び折損試験は実施例1と同様の方法にて実施し、その結果を同表中に示す。本発明の炭酸カルシウム粉末の平均粒径が0.5〜5μm、板状タルク粉末の平均板径が0.1〜5μmの範囲であれば、自己摩耗量10μm以下で且つ耐折損性が100%以上であった。
Examples 5 to 7 (J5 to 7) and Comparative Examples 4 to 6 (H4 to 6)
A test piece for wear test and a test piece for breakage test were carried out with the composition of the same blending ratio as in Example 2 (J2) with the particle diameters or plate diameters of calcium carbonate powder and plate-like talc powder as shown in Table 2 Prepared in the same manner as in Example 2 (J2). In Examples 5 and 6 (J5, 6) and Comparative Example 4 (H4), the powder-sized raw material of Example 2 (J2) was mixed and pulverized by changing the stirring conditions by high-speed stirring with a Henschel mixer. . The wear test and breakage test were performed in the same manner as in Example 1, and the results are shown in the same table. When the average particle diameter of the calcium carbonate powder of the present invention is in the range of 0.5 to 5 μm and the average plate diameter of the plate-like talc powder is in the range of 0.1 to 5 μm, the self-wear amount is 10 μm or less and the fracture resistance is 100% or more. .

Figure 0004589154
Figure 0004589154

実施例8(J8)
実施例2(J2)の配合割合の組成で、板状タルクの1/2(5重量%)を平均板径7μmの鱗片状黒鉛に置き換えて、実施例2と同じ方法で摩耗試験用テストピースと折損試験用テストピースを作製した。摩耗試験及び折損試験は実施例1と同様の方法にて実施し、その結果、自己摩耗量4μ、相手材摩耗量7μm、耐折損性100%で、特に相手攻撃性が著しく改善された。
Example 8 (J8)
A test piece for wear test in the same manner as in Example 2 except that 1/2 (5% by weight) of the plate-like talc is replaced with scaly graphite having an average plate diameter of 7 μm in the composition ratio of Example 2 (J2). A test piece for breakage test was prepared. The wear test and breakage test were carried out in the same manner as in Example 1. As a result, the self-abrasion amount was 4 μm, the counterpart material wear amount was 7 μm, and the breakage resistance was 100%.

実施例9〜12(J9〜12)
PEEK以外は実施例2(J2)と同じ配合割合の組成とし、実施例9(J9)ではPEEKの1/3(20重量%)をPENに置き換え、実施例10〜12(J10〜12)ではPEEKの全てをそれぞれPEN(J10)、PEK(J11)、PPS(J12)に置き換えて、実施例2と同じ方法で摩耗試験用テストピースと折損試験用テストピースを作製した。摩耗試験及び折損試験は実施例1と同様の方法にて実施し、その結果を表3に示す。その結果、選択された耐熱性エンジニアリングプラスチックはいずれもPEEKに置き換えても、本発明の目的を達成することができる。
Examples 9-12 (J9-12)
Except for PEEK, the composition was the same as in Example 2 (J2). In Example 9 (J9), 1/3 (20% by weight) of PEEK was replaced with PEN. In Examples 10 to 12 (J10 to 12) By replacing all of PEEK with PEN (J10), PEK (J11), and PPS (J12), respectively, a test piece for wear test and a test piece for breakage test were produced in the same manner as in Example 2. The wear test and breakage test were performed in the same manner as in Example 1, and the results are shown in Table 3. As a result, the object of the present invention can be achieved even if any selected heat-resistant engineering plastic is replaced with PEEK.

Figure 0004589154
Figure 0004589154

松原式摩耗試験機の要部概略断面図である。It is a principal part schematic sectional drawing of a Matsubara type abrasion tester. シールリング専用折損試験機の概略図である。It is the schematic of a seal ring exclusive use break test machine.

符号の説明Explanation of symbols

1 アルミ円板用ホルダー(固定)
2 シールリング用ホルダー(固定)
3 アルミ円板
4 評価用シールリング
5 オイルバス
6 オイル
7 オイル飛散防止カバー
1 Aluminum disc holder (fixed)
2 Holder for seal ring (fixed)
3 Aluminum disc 4 Seal ring for evaluation 5 Oil bath 6 Oil 7 Oil scattering prevention cover

Claims (3)

ポリエーテルエーテルケトン樹脂65重量%以下、平均繊維径3〜10μmの炭素繊維10〜30重量%、平均粒径0.5〜5μmの炭酸カルシウム粉末と平均板径0.1〜5μmの板状タルク粉末を合計10〜35重量%含有し、前記炭酸カルシウム粉末重量/前記板状タルク粉末重量比率が0.2〜1.2の範囲内にあることを特徴とする複合樹脂シールリング。 Polyetheretherketone resin 65 wt% or less, carbon fiber 10-30 wt% with an average fiber diameter 3-10 μm, calcium carbonate powder with an average particle diameter 0.5-5 μm and plate-like talc powder with an average plate diameter 0.1-5 μm in total 10 A composite resin seal ring comprising -35 wt% , wherein the calcium carbonate powder weight / plate talc powder weight ratio is in the range of 0.2 to 1.2 . 前記ポリエーテルエーテルケトンの一部又は全部をポリエーテルケトン、ポリエーテルニトリル、ポリフェニレンサルファイドからなる群から選ばれるいずれか一つの樹脂で置き換えることを特徴とする請求項1に記載の複合樹脂シールリング。 2. The composite resin seal ring according to claim 1, wherein a part or all of the polyether ether ketone is replaced with any one resin selected from the group consisting of polyether ketone, polyether nitrile, and polyphenylene sulfide. 前記炭酸カルシウム粉末と前記板状タルク粉末を乾式で高速撹拌によって均一に混合粉砕したことを特徴とする請求項1又は2に記載の複合樹脂シールリング。 The composite resin seal ring according to claim 1 or 2 , wherein the calcium carbonate powder and the plate-like talc powder are uniformly mixed and pulverized by high-speed stirring in a dry method.
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JPH05262976A (en) * 1991-12-25 1993-10-12 Ntn Corp Oil seal ring
JPH07179846A (en) * 1993-12-24 1995-07-18 Ntn Corp Oil seal ring
JPH11218219A (en) * 1998-01-29 1999-08-10 Riken Corp Seal ring
JP2002089718A (en) * 1994-06-30 2002-03-27 Ntn Corp Synthetic resin seal ring

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JPH05262976A (en) * 1991-12-25 1993-10-12 Ntn Corp Oil seal ring
JPH07179846A (en) * 1993-12-24 1995-07-18 Ntn Corp Oil seal ring
JP2002089718A (en) * 1994-06-30 2002-03-27 Ntn Corp Synthetic resin seal ring
JPH11218219A (en) * 1998-01-29 1999-08-10 Riken Corp Seal ring

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