JP2005201289A - Composite for dry lubrication coat film formation - Google Patents
Composite for dry lubrication coat film formation Download PDFInfo
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Abstract
Description
本発明は、自動車やその他の産業機械に使用される摺動部材に乾性潤滑被膜を形成するための組成物およびそれを使用した乾性潤滑被膜の製造方法に関する。 The present invention relates to a composition for forming a dry lubricating film on a sliding member used in automobiles and other industrial machines, and a method for producing a dry lubricating film using the composition.
すべり軸受用の乾性潤滑被膜としてこれまでに、ポリアミドイミド系樹脂などの熱硬化性樹脂を被膜形成剤として含有し、更に必要に応じて、二硫化モリブデン、グラファイトなどの固体潤滑剤、および／または、窒化ケイ素、アルミナなどの硬質粒子（摩擦調整剤）を含有する被膜が開示されている（特許文献１、特許文献２および特許文献３を参照されたい）。 As a dry lubricating film for a sliding bearing, a thermosetting resin such as a polyamide-imide resin has been included as a film forming agent, and if necessary, a solid lubricant such as molybdenum disulfide and graphite, and / or , A coating containing hard particles (friction modifier) such as silicon nitride and alumina is disclosed (see Patent Document 1, Patent Document 2 and Patent Document 3).
これらの乾性潤滑被膜はいずれも、熱硬化性樹脂、固体潤滑剤、硬質粒子を適当な有機溶媒に希釈した組成物（すなわち、乾性潤滑被膜形成用組成物）を予め調製し、該組成物を適当な化学的または物理的処理を施した母材（ワーク）に塗布し、乾燥し、焼成することにより製造される。 All of these dry lubricating coatings are prepared in advance by preparing a composition in which a thermosetting resin, a solid lubricant, and hard particles are diluted in an appropriate organic solvent (that is, a composition for forming a dry lubricating coating). It is manufactured by applying to a base material (work) subjected to appropriate chemical or physical treatment, drying and firing.
また、特許文献４には、乾性潤滑被膜形成用組成物を母材に塗布するときの発泡を抑制する目的で、乾性潤滑被膜形成用組成物中に特定のシリコーン消泡剤を添加する技術が開示されている。
従来の乾性潤滑被膜の形成方法では、被膜形成用組成物を塗布する前に母材を６０〜９０℃程度に予備加熱することが必要であり工程が複雑なものとなっていた。また、乾燥または焼成の工程で気泡や膨れが発生し易いという問題もあった。更にまた、乾性潤滑被膜形成用組成物の粘度が低いために印刷部分の周縁部（以下、「額縁部分」または「額縁」と称する）が大きく盛り上がり、摺動時に被膜欠損の原因となるという問題があった。なお特許文献４における特定のシリコーン消泡剤の添加は発泡を抑制することを目的とするものであり、被膜形成用組成物を塗布する前に母材を予備加熱することが必要であるという問題点は解決していない。 In the conventional method for forming a dry lubricating coating, it is necessary to preheat the base material to about 60 to 90 ° C. before applying the coating forming composition, and the process is complicated. There is also a problem that bubbles and blisters are likely to occur during the drying or firing process. Furthermore, since the viscosity of the composition for forming a dry lubricating coating is low, the peripheral portion of the printed portion (hereinafter referred to as “frame portion” or “frame”) greatly rises and causes a film defect during sliding. was there. The addition of a specific silicone antifoaming agent in Patent Document 4 is intended to suppress foaming, and it is necessary to preheat the base material before applying the film forming composition. The point is not solved.
本発明はこれらの問題点を解決することを目的とする。すなわち本発明は、乾性潤滑被膜形成に際して母材の予備加熱をする必要がなく、被膜に気泡や膨れが発生し難く、且つ、得られる乾性潤滑被膜の額縁部分の盛り上がりが少ない、乾性潤滑被膜形成用組成物を提供することを目的とする。 The present invention aims to solve these problems. That is, the present invention eliminates the need for preheating the base material when forming a dry lubricating film, makes it difficult for bubbles and blisters to occur in the film, and forms a dry lubricating film with little rise in the frame portion of the resulting dry lubricating film. It is an object to provide a composition for use.
（１）(a)成分：熱硬化性樹脂、(b)成分：固体潤滑剤および／または硬質粒子、(c)成分：前記(a)成分を溶解することができる溶媒、ならびに、(d)成分：一般式
で表されるポリエーテル変性シリコーンを含有し、前記(d)成分の含有量が、前記(a)成分を前記(c)成分に溶解させた場合に得られるワニスを１００体積部としたとき、０．０１〜０．４０体積部である、乾性潤滑被膜形成用組成物。
（２）上記（１）に記載の乾性潤滑被膜形成用組成物を母材に塗布し、塗布された該組成物に含まれる溶媒を除去した後、焼成することを含む乾性潤滑被膜の製造方法。
(1) Component (a): thermosetting resin, component (b): solid lubricant and / or hard particles, component (c): solvent capable of dissolving the component (a), and (d) Ingredient: General formula
When the content of the component (d) is 100 parts by volume of the varnish obtained when the component (a) is dissolved in the component (c), A composition for forming a dry lubricating film, which is 0.01 to 0.40 part by volume.
(2) A method for producing a dry lubricating film, comprising applying the composition for forming a dry lubricating film according to (1) to a base material, removing the solvent contained in the applied composition, and then baking the composition. .
本発明の乾性潤滑被膜形成用組成物は、乾性潤滑被膜形成に際して母材の予備加熱をする必要がなく、気泡や膨れが発生し難い。従って、本発明の組成物を使用することにより乾性潤滑被膜の製造が容易になる。また、本発明の組成物を使用すれば、額縁部分の盛り上がりが少ない乾性潤滑被膜を容易に製造することができる。 The composition for forming a dry lubricating film of the present invention does not require preliminary heating of the base material when forming the dry lubricating film, and bubbles and blisters are less likely to occur. Accordingly, the use of the composition of the present invention facilitates the production of a dry lubricating film. Moreover, if the composition of this invention is used, a dry lubricating film with few rises of a frame part can be manufactured easily.
以下、本発明を詳細に説明する。
本発明は、(a)成分：熱硬化性樹脂、(b)成分：固体潤滑剤および／または硬質粒子、(c)成分：前記(a)成分を溶解することができる溶媒、ならびに、(d)成分：一般式
で表されるポリエーテル変性シリコーンを含有し、前記(d)成分の含有量が、前記(a)成分を前記(c)成分に溶解させた場合に得られるワニスを１００体積部としたとき、０．０１〜０．４０体積部である、乾性潤滑被膜形成用組成物に関する。この組成物は、乾性潤滑被膜形成に際して母材の予備加熱をする必要がなく、気泡や膨れが発生し難い。従ってこの組成物を使用することにより乾性潤滑被膜の製造が容易になる。本発明の組成物はまた、(d)成分を含まない通常の乾性潤滑被膜形成用組成物と比較して粘度が高いため、この組成物を例えばスクリーン印刷によりすべり軸受の母材に塗布し乾燥・焼成した場合に印刷部分の額縁が盛り上がる程度が少なく、形成された被膜が摺動時に欠損しにくいという点でも有利である。
Hereinafter, the present invention will be described in detail.
The present invention comprises (a) component: thermosetting resin, (b) component: solid lubricant and / or hard particles, (c) component: a solvent capable of dissolving the component (a), and (d ) Component: General formula
When the content of the component (d) is 100 parts by volume of the varnish obtained when the component (a) is dissolved in the component (c), The present invention relates to a composition for forming a dry lubricating film that is 0.01 to 0.40 part by volume. In this composition, it is not necessary to preheat the base material when forming the dry lubricating film, and bubbles and swelling are hardly generated. Therefore, the use of this composition facilitates the production of a dry lubricating film. Since the composition of the present invention also has a higher viscosity than a normal dry lubricating film-forming composition not containing the component (d), the composition is applied to a base material of a plain bearing by, for example, screen printing and dried. -It is advantageous in that the frame of the printed portion is less raised when baked, and the formed film is less likely to be damaged during sliding.
本発明に使用できる熱硬化性樹脂としては、ポリイミド系樹脂、ポリアミドイミド系樹脂、エポキシ樹脂、フェノール樹脂等が挙げられる。熱硬化性樹脂は乾性潤滑被膜が形成されたときに、固体潤滑剤または硬質粒子を結合するとともに、軸によりけずられなじみ性を発揮し、さらに腐食に対して極めて安定である。 Examples of the thermosetting resin that can be used in the present invention include polyimide resins, polyamideimide resins, epoxy resins, and phenol resins. The thermosetting resin binds a solid lubricant or hard particles when a dry lubricating film is formed, exhibits shearing compatibility with the shaft, and is extremely stable against corrosion.
上記の熱硬化性樹脂を溶解できる溶媒（(c)成分）としては、例えばＮ−メチルピロリドン、Ｎ，Ｎ−ジメチルアセトアミドを挙げることができるがこれらには限られない。 Examples of the solvent capable of dissolving the thermosetting resin (component (c)) include, but are not limited to, N-methylpyrrolidone and N, N-dimethylacetamide.
本発明の乾性潤滑被膜形成用組成物の２５℃での粘度は通常は１０００〜３００００ｍＰａ・Ｓであるが、２０００〜１００００ｍＰａ・Ｓであればより好ましい。粘度が高すぎる場合は、適宜溶媒により希釈して所望の粘度に調整することができる。すなわち本発明の組成物中における上記(c)成分の添加量は、組成物の粘度が１０００〜３００００ｍＰａ・Ｓ、好ましくは２０００〜１００００ｍＰａ・Ｓとなる量であることが好ましい。 The viscosity at 25 ° C. of the composition for forming a dry lubricating film of the present invention is usually 1000 to 30000 mPa · S, more preferably 2000 to 10000 mPa · S. When the viscosity is too high, it can be adjusted to a desired viscosity by appropriately diluting with a solvent. That is, the addition amount of the component (c) in the composition of the present invention is preferably such an amount that the viscosity of the composition is 1000 to 30000 mPa · S, preferably 2000 to 10000 mPa · S.
本発明の乾性潤滑被膜形成用組成物は、(d)成分として一般式
で表されるポリエーテル変性シリコーンを含有する。その機構は明らかではないが実施例から示されるように、このポリエーテル変性シリコーンが添加されていることにより母材（ワーク）が室温程度（２５℃前後）に維持されている場合にも気泡や膨れの発生が抑制できるとともに、乾性潤滑被膜形成用組成物の粘度が適度に高くたもたれるためスクリーン印刷時の額縁部分の肥大化が抑制できる。また上記一般式において −(R'’−O)− で表されるポリエーテル基としては、エチレンオキサイドもしくはプロピレンオキサイド単独であっても、またはそれらが両者混在するものであってもよい。
The composition for forming a dry lubricating film of the present invention has a general formula as the component (d).
The polyether modified silicone represented by these is contained. Although the mechanism is not clear, as shown in the examples, even when the base material (work) is maintained at about room temperature (around 25 ° C.) by adding this polyether-modified silicone, The occurrence of blistering can be suppressed, and the viscosity of the composition for forming a dry lubricating film can be moderately increased, so that enlargement of the frame portion during screen printing can be suppressed. The polyether group represented by — (R ″ —O) — in the above general formula may be ethylene oxide or propylene oxide alone, or may be a mixture of both.
本発明の乾性潤滑被膜形成用組成物は通常、前記(a)成分（熱硬化性樹脂）を前記(c)成分（溶媒）に溶解させてワニスを得た後、上記の(c)成分および(d)成分ならびにその他の必要な成分を添加して調製するのであるが、この組成物中での上記ポリエーテル変性シリコーン（(d)成分）の含有量は、このワニスを１００体積部とした場合に０．０１〜０．４０体積部である。(d)成分の含有量が同０．０１体積部未満である場合には含有量が低すぎるために本発明の効果が得られず、また、(d)成分の含有量が同０．４０体積部を超える場合には乾性潤滑被膜形成用組成物を母材表面に塗布することが困難となり（例えば組成物が母材表面ではじかれる）本発明の効果が得られない。 The composition for forming a dry lubricating film of the present invention is usually obtained by dissolving the component (a) (thermosetting resin) in the component (c) (solvent) to obtain a varnish, The component (d) and other necessary components are added and prepared. The content of the polyether-modified silicone (component (d)) in the composition is 100 parts by volume of the varnish. In some cases, it is 0.01 to 0.40 parts by volume. When the content of component (d) is less than 0.01 parts by volume, the content is too low to achieve the effects of the present invention, and the content of component (d) is 0.40. When it exceeds the volume part, it becomes difficult to apply the composition for forming a dry lubricating film on the surface of the base material (for example, the composition is repelled on the surface of the base material), and the effect of the present invention cannot be obtained.
(b)成分としての固体潤滑剤としては、二硫化モリブデン（ＭｏＳ2）、グラファイト、窒化ホウ素（ＢＮ）、二硫化タングステン（ＷＳ2）、ポリテトラフルオロエチレン（ＰＴＦＥ）等のフッ素系樹脂、鉛（Ｐｂ）等を挙げることができる。グラファイトは天然、人造グラファイトのいずれでもよいが、人造グラファイトが耐摩耗性の観点から好ましい。これらの固体潤滑剤は、摩擦係数を低く且つ安定にする作用とともに、なじみ性を有する。これらの作用を十分に発揮させるために、固体潤滑剤の平均粒径は１５μｍ以下、特に０．２〜１０μｍであることが好ましい。(b)成分としての固体潤滑剤の好ましい添加量は(a)成分を１００体積部とした場合に１〜１０体積部、より好ましくは１〜５体積部である。 As the solid lubricant as component (b), fluorine-based resins such as molybdenum disulfide (MoS 2 ), graphite, boron nitride (BN), tungsten disulfide (WS 2 ), polytetrafluoroethylene (PTFE), lead (Pb) etc. can be mentioned. The graphite may be either natural or artificial graphite, but artificial graphite is preferred from the viewpoint of wear resistance. These solid lubricants have a conformability as well as a low and stable friction coefficient. In order to sufficiently exhibit these functions, the average particle diameter of the solid lubricant is preferably 15 μm or less, particularly preferably 0.2 to 10 μm. A preferable addition amount of the solid lubricant as the component (b) is 1 to 10 parts by volume, more preferably 1 to 5 parts by volume when the component (a) is 100 parts by volume.
(b)成分としての硬質粒子としては、酸化ケイ素（ＳｉＯ2）、酸化アルミニウム（Ａｌ2Ｏ3）、酸化クロム（ＣｒＯ2）、酸化チタン（ＴｉＯ2）、酸化亜鉛（ＺｒＯ2）、酸化鉄（Ｆｅ2Ｏ3）、ムライトなどの酸化物粒子の他にＳｉＣなどの炭化物，Ｓｉ3Ｎ4などの窒化物も使用することができる。これらの硬質粒子は最終的な乾式潤滑被膜の摩耗を抑制する摩擦調整剤として作用する。硬質粒子は使用される相手軸、通常は炭素鋼、合金鋼、鋳鉄、鋳鋼製軸より硬度が高いものであり、好ましい硬度はＨｖ２００以上、より好ましくはＨｖ６００以上である。但し、かかる硬質粒子とＺｎＯ，ＳｎＯ2などの軟質粒子の併用をしてもよい。軟質球形粒子は主としてなじみ性を発揮する。また、硬質粒子の粒径は平均で０．１〜５μｍ、特に２μｍ以下であることが好ましい。(b)成分としての硬質粒子の好ましい添加量は(a)成分を１００体積部とした場合に１〜１５体積部、より好ましくは１〜６体積部である。硬質粒子と熱硬化性樹脂との接着性を高めるために、硬質粒子表面をシランカップリング剤等により処理することができ、またＣｕ，Ｎｉめっきなどの金属表面処理や酸によるエッチングなどの無機物を用いた処理を行うこともできる。 As hard particles as component (b), silicon oxide (SiO 2 ), aluminum oxide (Al 2 O 3 ), chromium oxide (CrO 2 ), titanium oxide (TiO 2 ), zinc oxide (ZrO 2 ), iron oxide In addition to oxide particles such as (Fe 2 O 3 ) and mullite, carbides such as SiC and nitrides such as Si 3 N 4 can also be used. These hard particles act as a friction modifier that suppresses the wear of the final dry lubricating coating. The hard particles have a higher hardness than the counterpart shaft used, usually carbon steel, alloy steel, cast iron, or cast steel shaft, and the preferred hardness is Hv200 or higher, more preferably Hv600 or higher. However, such hard particles may be used in combination with soft particles such as ZnO and SnO 2 . Soft spherical particles are mainly compatible. The average particle size of the hard particles is preferably 0.1 to 5 μm, particularly preferably 2 μm or less. A preferable addition amount of the hard particles as the component (b) is 1 to 15 parts by volume, more preferably 1 to 6 parts by volume when the component (a) is 100 parts by volume. In order to improve the adhesion between the hard particles and the thermosetting resin, the surface of the hard particles can be treated with a silane coupling agent or the like, and inorganic materials such as metal surface treatments such as Cu and Ni plating and etching with acids can be used. The processing used can also be performed.
更にまた、本発明の乾性潤滑被膜形成用組成物は、形成される乾性潤滑被膜の用途に応じて上記(a)〜(d)成分以外にも種々の成分（膜形成助剤など）を適宜含有し得る。 Furthermore, the composition for forming a dry lubricating film of the present invention appropriately contains various components (film forming aids and the like) in addition to the above components (a) to (d) depending on the use of the dry lubricating film to be formed. May be contained.
含有し得る膜形成助剤としてはエポキシ樹脂またはエポキシシランが挙げられる。
エポキシ樹脂は、液状タイプのポリアミドイミド樹脂と相溶性が高い。エポキシ基は母材金属（例えばアルミニウム）表面になじみやすい。このため膜形成助剤としてエポキシ樹脂を用いると、ポリアミドイミド樹脂の母材金属表面への密着性を助けると共に、ポリアミドイミド樹脂との反応（ポリアミドイミド樹脂自体の縮合反応）により最終的な乾性潤滑被膜の耐摩耗性を向上させることができる。
Examples of the film forming aid that may be contained include epoxy resins and epoxy silanes.
The epoxy resin is highly compatible with the liquid type polyamideimide resin. Epoxy groups are easy to conform to the surface of the base metal (eg, aluminum). For this reason, using an epoxy resin as a film-forming aid helps the polyamideimide resin adhere to the base metal surface and at the same time provides a final dry lubrication by reaction with the polyamideimide resin (condensation reaction of the polyamideimide resin itself). The wear resistance of the coating can be improved.
膜形成助剤としてのエポキシ樹脂は、(a)成分を１００体積部とした場合に０．１〜１０体積部の範囲で添加するのが好ましい。添加量が０．１体積部未満であると上記の添加効果が認められないので好ましくない。また添加量が１０体積部を超えると耐摩耗性および密着性を逆に低下させるので好ましくない。 The epoxy resin as the film forming aid is preferably added in the range of 0.1 to 10 parts by volume when the component (a) is 100 parts by volume. If the addition amount is less than 0.1 part by volume, the above-described addition effect is not recognized, which is not preferable. On the other hand, if the amount added exceeds 10 parts by volume, the wear resistance and adhesion are reduced, which is not preferable.
エポキシシランは、固体潤滑剤または硬質粒子のポリアミドイミド樹脂に対する分散性を向上させることができる。すなわち、エポキシシランは液状で無機構造を有しているためアルミナなどの無機固体と親和性が高く、また有機基を有しているためポリアミドイミド樹脂との相溶性も高いため、膜形成助剤としてエポキシシランを用いると、ポリアミドイミド樹脂に対する無機固体の分散性が向上する。さらにまた、エポキシシランもまたエポキシ基を有しているためポリアミドイミド樹脂の母材金属表面への密着性を向上させることができる。 Epoxysilane can improve the dispersibility of the solid lubricant or hard particles in the polyamideimide resin. That is, epoxy silane is liquid and has an inorganic structure, so it has high affinity with inorganic solids such as alumina, and since it has an organic group, it is highly compatible with polyamide-imide resin. When epoxy silane is used, the dispersibility of the inorganic solid with respect to the polyamide-imide resin is improved. Furthermore, since the epoxy silane also has an epoxy group, the adhesion of the polyamide-imide resin to the base metal surface can be improved.
膜形成助剤としてのエポキシシランは、(a)成分を１００体積部とした場合に０．１〜５体積部の範囲で添加するのが好ましい。添加量が０．１体積部未満であると上記の添加効果が認められないので好ましくない。また添加量が５体積部を超えると効果が得られなくなるので好ましくない。 The epoxy silane as a film forming aid is preferably added in the range of 0.1 to 5 parts by volume when the component (a) is 100 parts by volume. If the addition amount is less than 0.1 part by volume, the above-described addition effect is not recognized, which is not preferable. Moreover, since an effect will no longer be acquired when addition amount exceeds 5 volume parts, it is unpreferable.
本発明はまた、上記の乾性潤滑被膜形成用組成物を母材に塗布し、塗布された該組成物に含まれる溶媒を除去した後、焼成することを含む乾性潤滑被膜の製造方法に関する。 The present invention also relates to a method for producing a dry lubricating film, which comprises applying the above composition for forming a dry lubricating film to a base material, removing the solvent contained in the applied composition, and then baking.
ここで母材は、摺動部材の基材となり得るものであれば任意の材質のものであってよく、例えばアルミニウム系合金、銅系合金などの金属、樹脂などが挙げられる。 Here, the base material may be any material as long as it can serve as a base material for the sliding member, and examples thereof include metals such as aluminum alloys and copper alloys, and resins.
摺動部材の基材としての合金は、特に組成が限定されないが、アルミニウム系合金としては、好ましくは１０重量％以下のＣｒ、Ｓｉ、Ｍｎ、Ｓｂ、Ｓｒ、Ｆｅ、Ｎｉ、Ｍｏ、Ｔｉ、Ｗ、Ｚｒ、Ｖ、Ｃｕ、Ｍｇ、Ｚｎなどと、２０重量％以下のＳｎ、Ｐｂ、Ｉｎ、Ｔｌ、Ｂｉの１種又は２種以上を含有する合金を好ましく使用することができる。前者の群の元素は主として強度、耐摩耗性を付与し、後者の群の元素は主としてなじみ性を付与する。前者と後者を組み合わせて使用することが好ましい。 The composition of the alloy as the base material of the sliding member is not particularly limited, but as an aluminum-based alloy, preferably Cr, Si, Mn, Sb, Sr, Fe, Ni, Mo, Ti, W of 10% by weight or less are preferable. , Zr, V, Cu, Mg, Zn, and the like, and an alloy containing 20% by weight or less of Sn, Pb, In, Tl, Bi or more can be preferably used. The former group of elements mainly provides strength and wear resistance, and the latter group of elements mainly provides compatibility. It is preferable to use the former and the latter in combination.
またこれらに限らず本発明の乾性潤滑被膜形成用組成物はピストン、ピストンリング、シム、クラッチ等の潤滑条件下、無潤滑条件下を含め様々な用途の部材に幅広く適用可能である。 In addition, the composition for forming a dry lubricating coating of the present invention is not limited to these, and can be widely applied to members for various uses including lubricating conditions such as pistons, piston rings, shims, and clutches, and non-lubricating conditions.
母材は塗布に先立ち以下のよう処理するのが好ましい。銅合金、アルミニウム合金、樹脂等の母材を摺動部形状に加工した後、苛性ソーダなどのアルカリ処理液中で脱脂処理し、続いて水洗及び湯洗を行い表面に付着したアルカリを除去する。例えば、乾性潤滑被膜の密着性を高くする必要があるとき、脱脂後アルカリエッチングと酸洗との組合せ等の化学的処理により母材の表面を粗面化する、ショットブラストなどの機械的処理により母材表面を粗面化する、ボーリング加工等により母材表面に凹凸を形成する等の方法をとることができる。更に密着性を高める必要があるときは、母材表面に厚さ０．１〜５μｍのリン酸亜鉛又はリン酸亜鉛カルシウム化成処理を施してもよい。ボーリングなどの下地処理と化成処理を組み合わせると、極めて密着性が高い乾性潤滑被膜が得られる。 Prior to application, the base material is preferably treated as follows. After a base material such as a copper alloy, an aluminum alloy, or a resin is processed into a sliding part shape, it is degreased in an alkali treatment liquid such as caustic soda, followed by washing with water and hot water to remove the alkali attached to the surface. For example, when it is necessary to increase the adhesion of the dry lubricating film, the surface of the base material is roughened by chemical treatment such as a combination of alkaline etching and pickling after degreasing, by mechanical treatment such as shot blasting. Methods such as roughening the surface of the base material or forming irregularities on the surface of the base material by boring or the like can be employed. When it is necessary to further improve the adhesion, the surface of the base material may be subjected to a zinc phosphate or zinc phosphate calcium chemical conversion treatment having a thickness of 0.1 to 5 μm. When a base treatment such as boring is combined with a chemical conversion treatment, a dry lubricating coating with extremely high adhesion can be obtained.
本発明の乾性潤滑被膜形成用組成物を母材に塗布する方法は種々のものがある。例えば実施例に示すようにスクリーン印刷法により塗布することができる。その他にスプレー法、タンブリング法、浸漬法、刷毛塗り法などにより塗布することもできる。形成される乾性潤滑被膜の厚みは１〜５０μｍであることが好ましい。スクリーン印刷法により本発明の組成物を母材に塗布する場合は、剣スキージを使用することにより乾性潤滑被膜の厚みを８〜２０μｍにすることが容易である。なお、上記の通り本発明の乾性潤滑被膜形成用組成物を使用すれば母材を予備加熱する必要はなく、室温（２５℃前後）下にて母材に塗布すればよい。ただしより好ましい被膜を得るために母材を予備加熱することもできる。 There are various methods for applying the composition for forming a dry lubricating film of the present invention to a base material. For example, it can be applied by screen printing as shown in the examples. In addition, it can be applied by spraying, tumbling, dipping, brushing, or the like. The thickness of the dry lubricating film formed is preferably 1 to 50 μm. When the composition of the present invention is applied to the base material by a screen printing method, it is easy to make the dry lubricating coating thickness 8 to 20 μm by using a sword squeegee. As described above, if the composition for forming a dry lubricating film of the present invention is used, it is not necessary to preheat the base material, and it may be applied to the base material at room temperature (around 25 ° C.). However, the base material can be preheated to obtain a more preferable film.
本発明の乾性潤滑被膜形成用組成物を母材に塗布した後、一定時間レベリングを行うことが好ましい。レベリングにより、形成される乾性潤滑被膜の潤滑性が向上する。 After applying the composition for forming a dry lubricating film of the present invention to a base material, it is preferable to perform leveling for a certain time. Leveling improves the lubricity of the dry lubricating coating formed.
本発明の乾性潤滑被膜形成用組成物を母材に塗布した後に、好ましくは更にレベリングを行った後に、母材に塗布された組成物に含まれる溶媒（(c)成分）を除去する。例えば８０〜９０℃にて１０〜３０分間加熱することにより溶媒を除去する。 After the composition for forming a dry lubricating film of the present invention is applied to a base material, preferably after further leveling, the solvent (component (c)) contained in the composition applied to the base material is removed. For example, the solvent is removed by heating at 80 to 90 ° C. for 10 to 30 minutes.
溶媒を除去した後に更に焼成を行う。焼成は、例えば１７０〜２００℃にて９０〜１２０分間加熱することにより行う。焼成を行うことで熱硬化性樹脂が強固な被膜を形成する。なお、条件が適当であれば、上記の溶媒の除去と焼成とを同時に行うことも可能である。 Further baking is performed after the solvent is removed. Firing is performed, for example, by heating at 170 to 200 ° C. for 90 to 120 minutes. By performing the baking, the thermosetting resin forms a strong film. If the conditions are appropriate, the removal of the solvent and the firing can be performed simultaneously.
乾性潤滑被膜形成用組成物の調製
ポリアミドイミド樹脂（日立化成株式会社製、分子量１４５００）１００体積部とエポキシ樹脂（油化シェルエポキシ株式会社製、エピコート８２８）０．８体積部とを、Ｎ−メチルピロリドン７５体積部およびＮ，Ｎ−ジメチルアセトアミド７５体積部に溶解してワニスを得た。
Preparation of a composition for forming a dry lubricating coating 100 parts by volume of polyamideimide resin (manufactured by Hitachi Chemical Co., Ltd., molecular weight 14500) and 0.8 part by volume of epoxy resin (manufactured by Yuka Shell Epoxy Co., Ltd., Epicoat 828) are mixed with N- A varnish was obtained by dissolving in 75 parts by volume of methylpyrrolidone and 75 parts by volume of N, N-dimethylacetamide.
上記ワニス１００体積部に、平均粒径０．６μｍのアルミナ粉３体積部、エポキシシラン（γ-グリンドプロピルトリメトキシシラン）１．２体積部およびカーボンブラック０．４体積部を添加して混合した。この混合物を三本ロールに２回通した後、この混合物中に表１に示す各種添加剤を表２に示す所定量だけ添加した。その後、Ｎ−メチルピロリドン５〜１５体積部を適宜添加して２５℃での粘度がいずれも３０００〜５０００ｍＰａ・Ｓになるように調整した。こうして各種乾性潤滑被膜形成用組成物を得た。 To 100 parts by volume of the varnish, 3 parts by volume of alumina powder having an average particle size of 0.6 μm, 1.2 parts by volume of epoxy silane (γ-glydopropyltrimethoxysilane) and 0.4 parts by volume of carbon black are added and mixed. did. After passing this mixture through three rolls twice, various additives shown in Table 1 were added to the mixture by a predetermined amount shown in Table 2. Thereafter, 5 to 15 parts by volume of N-methylpyrrolidone was appropriately added, and the viscosity at 25 ° C. was adjusted to 3000 to 5000 mPa · S. Thus, various dry lubricating film forming compositions were obtained.
スクリーン印刷性の試験
ワークとしてのピストンに上記の各種乾性潤滑被膜形成用組成物をスクリーン印刷法により印刷して乾性潤滑被膜を製造し評価した。
Various dry lubricating film forming compositions described above were printed on a piston as a screen-printing test workpiece by a screen printing method to produce and evaluate a dry lubricating film.
１６５メッシュスクリーンと硬度７０の剣スキージ（ウレタン製、スキージとスクリーンとの接触角度：９０°）を用い、スキージ速度２００ｍｍ／秒でスクリーン印刷法により、表２に示す各温度に維持したピストンに、上記の各種乾性潤滑被膜形成用組成物を印刷した。なお上記ピストンは、アルミニウム合金（ＡＣ８Ａ−Ｔ６）製で、表面粗さ１１Ｒｚであって、切削加工にて溝幅１５０〜３００μｍピッチ、深さ７〜１６μｍで条痕が設けられており、アルカリ脱脂処理が施されているものを使用した。 Using a 165 mesh screen and a sword squeegee with a hardness of 70 (urethane, contact angle between the squeegee and the screen: 90 °), a piston maintained at each temperature shown in Table 2 by screen printing at a squeegee speed of 200 mm / sec. The various dry lubricating film forming compositions described above were printed. The piston is made of an aluminum alloy (AC8A-T6), has a surface roughness of 11 Rz, and is provided with striations with a groove width of 150 to 300 μm and a depth of 7 to 16 μm by cutting. What was processed was used.
印刷後、２分間室温にてレベリングを行った。続いて９０℃にて３０分間乾燥させて溶媒であるＮ−メチルピロリドンおよびＮ，Ｎ−ジメチルアセトアミドを除去した後、１８０℃にて９０分間焼成した。こうして、ワーク上に乾性潤滑被膜を形成した。 After printing, leveling was performed at room temperature for 2 minutes. Subsequently, after drying at 90 ° C. for 30 minutes to remove N-methylpyrrolidone and N, N-dimethylacetamide as solvents, baking was performed at 180 ° C. for 90 minutes. Thus, a dry lubricating film was formed on the workpiece.
得られた被膜の外観を観察するとともに、膜厚および額縁の高さを測定した。以下の表１には実施例および比較例に使用した各種添加物を示し、表２には各添加物の添加量とスクリーン印刷性試験の結果を示す。 While observing the appearance of the obtained film, the film thickness and the height of the frame were measured. Table 1 below shows various additives used in Examples and Comparative Examples, and Table 2 shows the amount of each additive added and the results of a screen printability test.
上記の通り、本発明の乾性潤滑被膜形成用組成物を使用した実施例１〜６ではワーク温度が室温の場合であっても形成される乾性潤滑被膜に気泡や膨れが観察されなかった。また比較例１と比較して額縁部分の高さが低かった。 As described above, in Examples 1 to 6 using the composition for forming a dry lubricating film of the present invention, no bubbles or blisters were observed in the formed dry lubricating film even when the workpiece temperature was room temperature. Further, the height of the frame portion was lower than that of Comparative Example 1.
Claims (2)
で表されるポリエーテル変性シリコーンを含有し、前記(d)成分の含有量が、前記(a)成分を前記(c)成分に溶解させた場合に得られるワニスを１００体積部としたとき、０．０１〜０．４０体積部である、乾性潤滑被膜形成用組成物。 Component (a): thermosetting resin, component (b): solid lubricant and / or hard particles, component (c): solvent capable of dissolving the component (a), and component (d): general formula
When the content of the component (d) is 100 parts by volume of the varnish obtained when the component (a) is dissolved in the component (c), A composition for forming a dry lubricating film, which is 0.01 to 0.40 part by volume.
A method for producing a dry lubricating film, comprising applying the composition for forming a dry lubricating film according to claim 1 to a base material, removing the solvent contained in the applied composition, and then baking.
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