WO2011024941A2 - Cu基焼結摺動部材 - Google Patents
Cu基焼結摺動部材 Download PDFInfo
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- WO2011024941A2 WO2011024941A2 PCT/JP2010/064565 JP2010064565W WO2011024941A2 WO 2011024941 A2 WO2011024941 A2 WO 2011024941A2 JP 2010064565 W JP2010064565 W JP 2010064565W WO 2011024941 A2 WO2011024941 A2 WO 2011024941A2
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- based sintered
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0425—Copper-based alloys
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/105—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing inorganic lubricating or binding agents, e.g. metal salts
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F3/26—Impregnating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0084—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ carbon or graphite as the main non-metallic constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0089—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with other, not previously mentioned inorganic compounds as the main non-metallic constituent, e.g. sulfides, glass
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
- C22C9/02—Alloys based on copper with tin as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
- C22C9/06—Alloys based on copper with nickel or cobalt as the next major constituent
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16C—SHAFTS; FLEXIBLE SHAFTS; ELEMENTS OR CRANKSHAFT MECHANISMS; ROTARY BODIES OTHER THAN GEARING ELEMENTS; BEARINGS
- F16C33/00—Parts of bearings; Special methods for making bearings or parts thereof
- F16C33/02—Parts of sliding-contact bearings
- F16C33/04—Brasses; Bushes; Linings
- F16C33/06—Sliding surface mainly made of metal
- F16C33/12—Structural composition; Use of special materials or surface treatments, e.g. for rust-proofing
- F16C33/121—Use of special materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/10—Copper
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2302/00—Metal Compound, non-Metallic compound or non-metal composition of the powder or its coating
- B22F2302/40—Carbon, graphite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2302/00—Metal Compound, non-Metallic compound or non-metal composition of the powder or its coating
- B22F2302/45—Others, including non-metals
Definitions
- the present invention relates to a Cu-based sintered sliding member, and more particularly to a Cu-based sintered sliding member that can cope with a high load environment.
- the sintered sliding member cannot be used because it exceeds the operating load range, and the Fe-Cu sintered sliding member having higher hardness and strength than the Cu-based sintered sliding member contains Fe. Since the Fe-based material is used for the shaft, there is a low possibility that abnormal friction or seizure due to the tomo-gael phenomenon will occur, and there is a problem that the reliability as the sliding member is insufficient. Therefore, there has been a demand for a Cu-based sintered sliding member that is less expensive than an expensive ball bearing and can be used in a higher load environment than before.
- a Cu-based sintered alloy having a seizure property (for example, Patent Document 1) is disclosed.
- the Cu-based sintered alloy of the prior art is a Cu—Ni—Sn alloy having a composition that causes spinodal decomposition by aging treatment.
- spinodal decomposition a fine structure is formed and the substrate is strengthened, and the substrate is in close contact with it.
- NiS hard particles and MoS 2 as a solid lubricant, wear resistance and seizure resistance are imparted in an environment of high temperature, high load, and low lubrication.
- the Ni-based hard particles used in the prior art are expensive, and the Ni-based hard particles contain Cr. Therefore, vacuum sintering is required, so the manufacturing cost is high and the cost merit is insufficient. It was.
- an object of the present invention is to provide a Cu-based sintered sliding member that does not require the addition of expensive hard particles and can be used in a high-load use environment.
- the invention of claim 1 contains 5 to 30% by mass of Ni, 5 to 20% by mass of Sn, and 0.1 to 1.2% by mass of P, with the balance being Cu and inevitable impurities.
- At least one or more of graphite, fluorinated graphite, molybdenum disulfide, tungsten disulfide, boron nitride, calcium fluoride, talc, and magnesium silicate mineral powder is used as the solid lubricant. It contains 3 to 10% by mass.
- the Cu—Ni—Sn-based alloy uses the property that it hardens by aging treatment, and the addition of P to the alloy further increases the strength of the alloy base, and more than Ni and P than the base.
- Ni-P-Cu-Sn alloy phase having a high concentration of Sn and Sn is present at the grain boundary, so that excellent wear resistance is obtained, and expensive hard particles are not required, resulting in low cost and high load.
- a Cu-based sintered sliding member that can be used in a bearing use environment can be obtained.
- Solid lubricants include graphite, fluorinated graphite, molybdenum disulfide, tungsten disulfide, boron nitride, calcium fluoride, talc (Mg 3 SiO 4 (OH) 2 ), and magnesium silicate (MgSiO 3 ) mineral powder.
- the present invention utilizes the property that a Cu—Ni—Sn based alloy is hardened by an aging treatment, and further increases the strength of the alloy base by adding P to the alloy, and further increases the strength of Ni, P and Sn over the base.
- Ni-P-Cu-Sn alloy phase with high concentration is present at the grain boundary, resulting in excellent wear resistance, low cost because expensive hard particles are unnecessary, and high load bearing use
- a Cu-based sintered sliding member that can be used in an environment can be obtained. Furthermore, wear resistance can be improved by adding a solid lubricant.
- Ni 5 to 30% by mass
- Ni forms a solid solution of P, Sn, and Cu and improves the strength of the sintered alloy by age hardening. Furthermore, the alloy phase having a higher concentration of Ni, P, and Sn than the base is present at the grain boundaries, thereby contributing to improvement in wear resistance.
- the amount of Ni necessary for obtaining hardening by aging treatment is not less than 5% by mass, and even if an amount exceeding 30% by mass is added, improvement in hardening by aging treatment is not recognized, and on the contrary, the raw material cost increases, which is not preferable. .
- Sn 5 to 20% by mass Sn forms a solid solution of Ni, P, and Cu and improves the strength of the sintered alloy by age hardening. Furthermore, the alloy phase having a higher concentration of Ni, P, and Sn than the base is present at the grain boundaries, thereby contributing to improvement in wear resistance. It is necessary to add 5% by mass or more of Sn necessary for obtaining hardening by aging treatment, and even if an amount exceeding 20% by mass is added, improvement in curing by aging treatment is not recognized, and on the other hand, attacking the opponent Is unfavorable because of the high.
- (C) P 0.1 to 1.2% by mass P improves the sinterability and forms a solid solution of Ni, Sn, and Cu and improves the strength of the sintered alloy. Furthermore, the alloy phase having a higher concentration of Ni, P, and Sn than the base is present at the grain boundaries, thereby contributing to wear resistance. If the P content is less than 0.1% by mass, the predetermined wear resistance cannot be obtained. On the other hand, if the P content exceeds 1.2% by mass, the aggression on the sliding mating material is increased and the mating material is worn. It is not preferable.
- Solid lubricant 0.3 to 10% by mass At least one of graphite, fluorinated graphite, molybdenum disulfide, tungsten disulfide, boron nitride, calcium fluoride, talc (Mg 3 SiO 4 (OH) 2 ), and magnesium silicate (MgSiO 3 ) mineral powder as a solid lubricant More than 0.3 to 10% by mass can be contained, and if the solid lubricant content is less than 0.3% by mass, the effect of improving the wear resistance cannot be obtained. Since it falls remarkably, it is not preferable.
- graphite and fluorinated graphite exist as free graphite and free fluorinated graphite dispersed and distributed in the substrate, imparting excellent lubricity to the sintered alloy, thereby contributing to improvement in wear resistance of the sintered alloy.
- molybdenum disulfide, tungsten disulfide, boron nitride, calcium fluoride, talc (Mg 3 SiO 4 (OH) 2 ), magnesium silicate (MgSiO 3 ) mineral powder imparts excellent lubricity to the sintered alloy.
- the metal contact between the sliding members is reduced, thereby contributing to the improvement of the wear resistance of the sintered alloy.
- Talc becomes enstatite after sintering.
- raw material powder is filled into a mold having a required shape and compacted to obtain a molded body having a required density.
- This molded body is sintered in a reducing atmosphere to obtain a sintered alloy.
- This sintered alloy is sized with a mold so as to satisfy the dimensional accuracy of the product.
- the size, density, hardness, strength, etc. of the sintered alloy after sizing are inspected, and those that pass the inspection are regarded as products.
- a bearing as a sliding member is exemplified.
- Ni atomized powder, graphite powder having an average particle diameter of 20 ⁇ m, molybdenum disulfide powder having an average particle diameter of 150 ⁇ m or less, calcium fluoride powder having an average particle diameter of 60 ⁇ m, and talc having an average particle diameter of 20 ⁇ m as a solid lubricant to be added Powder was prepared.
- Each of the Cu-based sintered alloys is impregnated with synthetic oil, and each of them has dimensions of outer diameter: 18 mm ⁇ inner diameter: 8 mm ⁇ height: 8 mm.
- Slidable member hereinafter referred to as the present invention example
- Cu-based sintered sliding member of the composition component that deviates from the invention and Cu-based sintered sliding member which is not attached to P as a comparison hereinafter, referred to as comparative example
- the thus obtained Cu-based sintered sliding member has pores dispersed in the substrate at a rate of 5 to 25% by mass.
- Table 1 shows Invention Examples 1 to 4, Comparative Examples 1 to 8, and Conventional Examples 1 to 2, and Table 2 shows Invention Examples 5 to 13 and Comparative Examples 9 to 13.
- Pressure ring test A ring-shaped test piece comprising Invention Examples 1 to 13, Comparative Examples 1 to 13 and Conventional Examples 1 and 2 was loaded in the radial direction, and the crushing load when the ring-shaped test piece was broken was measured to calculate the strength. did. The results are shown in the column of “crushing strength” in Tables 1 and 2.
- Abrasion resistance test An S45C shaft is inserted into a ring-shaped test piece comprising Invention Examples 1 to 13, Comparative Examples 1 to 12 and Conventional Examples 1 to 2, and a ring-shaped test piece comprising Invention Examples 1 to 13 and Comparative Examples 1 to 13 Rotating the shaft at 75 m / min for 1000 hours while applying a load from the outside of the ring-shaped test piece so that the surface pressure is 1.5 MPa in the radial direction (perpendicular to the axial direction of the shaft) The maximum wear depth on the sliding surface of each of the ring-shaped test piece and the S45C shaft after the test was measured, and the wear resistance was evaluated. The results are shown in Tables 1 and 2.
- the conditions performed in this abrasion resistance test are those under a high load environment.
- the ring-shaped test pieces made of the examples of the present invention both have excellent wear resistance because the maximum wear depth is smaller than the ring-shaped test pieces made of the comparative example and the conventional example. It can be seen that
- Comparative Examples 1 to 13 having a component composition outside the scope of the present invention that the ring-shaped test piece is inferior in at least one of the strength, the wear resistance, and the aggressiveness to the mating shaft material.
- Comparative Example 6 in which Ni exceeds 30% by mass, the maximum wear depth and the maximum wear depth of the counterpart shaft material are larger than those of the present invention example, and in Comparative Example 7 in which Sn is less than 5% by mass, Compared with the example of the present invention, the maximum wear depth increases, and in Comparative Example 7 where Sn exceeds 20% by mass, the maximum wear depth of the counterpart shaft material increases compared to the example of the present invention. Further, Comparative Examples 1, 2, 3, 5 and 7 are inferior in crushing strength as compared with the inventive examples.
- Comparative Example 9 in which P is less than 0.1% by mass, Comparative Examples 10 to 12 in which the solid lubricant exceeds 10% by mass, solid lubricant exceeds 10% by mass and P is 1.2% by mass In Comparative Example 13 exceeding%, the crushing strength is inferior to that of the inventive example, and the maximum wear depth is increased.
- Ni, P, Sn, and Cu in the alloy phase in which the concentration of Ni, P, and Sn existing in the grain boundary of the metal structure is higher than the average concentration of Ni, P, and Sn in the entire alloy Analysis was performed using an electron beam microanalyzer (EPMA). The results are shown in Table 3, and as an example of the analyzed alloy phase, an electron micrograph (COMPO image) is shown in FIG.
- the EPMA analysis conditions were an acceleration voltage of 15 kV, a beam diameter set to ⁇ 1 ⁇ m, and five grain boundary alloy phases shown in FIG. 1 were measured. The averaged values are listed in Table 3. From the analysis result by EPMA, the alloy of Inventive Example 1 has an alloy phase in which the concentrations of Ni, P and Sn are higher than the average concentration of Ni, P and Sn in the whole sintered alloy at the grain boundaries. I understand that.
- this invention is not limited to the said embodiment, A various deformation
- the bearing having the sliding surface on the inner periphery is exemplified as the sliding member, but the present invention can also be applied to other sliding members having the sliding surface.
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- Mechanical Engineering (AREA)
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- Organic Chemistry (AREA)
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Abstract
Description
(a)Ni:5~30質量%
Niは、P、Sn、Cuと素地の固溶体を形成し、時効硬化によって焼結合金の強度を向上させる。さらに素地よりもNi、P、Snの濃度が高い合金相を粒界に存在させることで、耐摩耗性向上に寄与する。時効処理による硬化を得るために必要なNi量は5質量%以上で、30質量%を超える量を添加しても時効処理による硬化の向上は認められなくなり、かえって原料コストが高くなるので好ましくない。
(b)Sn:5~20質量%
Snは、Ni、P、Cuと素地の固溶体を形成し、時効硬化によって焼結合金の強度を向上させる。さらに素地よりもNi、P、Snの濃度が高い合金相を粒界に存在させることで、耐摩耗性向上に寄与する。時効処理による硬化を得るために必要なSn量は5質量%以上添加することが必要で、20質量%を超える量を添加しても時効処理による硬化の向上は認められなくなり、かえって相手攻撃性が高くなるので好ましくない。
(c)P:0.1~1.2質量%
Pは、焼結性を向上させ、Ni、Sn、Cuと素地の固溶体を形成して、焼結合金の強度を向上させる。さらに、素地よりもNi、P、Snの濃度が高い合金相を粒界に存在させることで、耐摩耗性に寄与する。P含有量が0.1質量%未満では所定の耐摩耗性が得られず、一方、1.2質量%を越えると摺動相手材への攻撃性が高まり、相手材を磨耗させてしまうので好ましくない。
(d)固体潤滑剤:0.3~10質量%
固体潤滑剤として、黒鉛、フッ化黒鉛、二硫化モリブデン、二硫化タングステン、窒化ホウ素、フッ化カルシウム、タルク(Mg3SiO4(OH)2)、珪酸マグネシウム(MgSiO3)鉱物粉末のうち少なくとも1種類以上を0.3~10質量%含有することができ、固体潤滑剤の含有量が0.3質量%未満では耐摩耗性の向上効果が得られず、10質量%を超えると、強度が著しく低下するので好ましくない。
原料粉末に、粒径-100meshの電解Cu粉末と、粒径-250meshのSnアトマイズ粉末と、粒径-200meshのCu-8質量%Pアトマイズ粉末と、粒径250meshのCu-30質量%Niアトマイズ粉末と、添加する固体潤滑剤として平均粒径:20μmの黒鉛粉末、平均粒径:150μm以下の二硫化モリブデン粉末、平均粒径60μmのフッ化カルシウム粉末、平均粒径:20μmのタルクの粉末を用意した。
本発明例1~13、比較例1~13、従来例1~2からなるリング状試験片を半径方向から荷重をかけ、リング状試験片が破壊したときの圧環荷重を測定し、強度を算出した。その結果を表1および表2の「圧環強度」の欄に示した。
本発明例1~13、比較例1~12および従来例1~2からなるリング状試験片にS45Cのシャフトを挿入し、本発明例1~13、比較例1~13からなるリング状試験片の半径方向(シャフトの軸方向に対して直角方向)に面圧:1.5MPaとなるように荷重を前記リング状試験片の外側からかけながら前記シャフトを75m/minで1000時間回転させて試験を実施し、試験後のリング状試験片及びS45Cシャフトのそれぞれの摺動面における最大摩耗深さを測定し、耐摩耗性を評価した。その結果を表1および表2に記載した。
Claims (2)
- 5~30質量%のNiと、5~20質量%のSnと、0.1~1.2質量%のPとを含有し、残部がCu及び不可避不純物からなる時効硬化したCu基焼結摺動部材であって、金属組織の粒界に前記Niと前記Pと前記Snの濃度が前記摺動部材全体における前記Niと前記Pと前記Snの平均濃度よりも高い合金相が存在することを特徴とするCu基焼結摺動部材。
- 固体潤滑剤として、黒鉛、フッ化黒鉛、二硫化モリブデン、二硫化タングステン、窒化ホウ素、フッ化カルシウム、タルク、珪酸マグネシウム鉱物粉末のうち少なくとも1種類以上を0.3~10質量%含有することを特徴とする請求項1記載のCu基焼結摺動部材。
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
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US13/390,883 US20120145284A1 (en) | 2009-08-31 | 2010-08-27 | Cu-BASED SINTERED SLIDING MEMBER |
CN201080033183.7A CN102471832B (zh) | 2009-08-31 | 2010-08-27 | Cu基烧结滑动部件 |
US14/520,479 US9849511B2 (en) | 2009-08-31 | 2014-10-22 | Method of producing a Cu-based sintered sliding member |
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JP2009201072A JP5684977B2 (ja) | 2009-08-31 | 2009-08-31 | Cu基焼結摺動部材 |
JP2009-201072 | 2009-08-31 |
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US13/390,883 A-371-Of-International US20120145284A1 (en) | 2009-08-31 | 2010-08-27 | Cu-BASED SINTERED SLIDING MEMBER |
US14/520,479 Division US9849511B2 (en) | 2009-08-31 | 2014-10-22 | Method of producing a Cu-based sintered sliding member |
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WO2011024941A2 true WO2011024941A2 (ja) | 2011-03-03 |
WO2011024941A3 WO2011024941A3 (ja) | 2011-04-28 |
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WO2016035880A1 (ja) * | 2014-09-04 | 2016-03-10 | 株式会社ダイヤメット | Cu基焼結軸受及びCu基焼結軸受の製造方法 |
US10532406B2 (en) | 2014-09-11 | 2020-01-14 | Diamet Corporation | Sintered sliding member having exceptional corrosion resistance, heat resistance, and wear resistance; and method for producing said member |
US10941465B2 (en) | 2016-03-04 | 2021-03-09 | Diamet Corporation | Cu-based sintered sliding material, and production method therefor |
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JP2013023707A (ja) * | 2011-07-18 | 2013-02-04 | Fukuda Metal Foil & Powder Co Ltd | 粉末冶金用混合粉末 |
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Also Published As
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JP2011052252A (ja) | 2011-03-17 |
US20120145284A1 (en) | 2012-06-14 |
JP5684977B2 (ja) | 2015-03-18 |
US20150037196A1 (en) | 2015-02-05 |
CN102471832A (zh) | 2012-05-23 |
CN102471832B (zh) | 2014-07-30 |
US9849511B2 (en) | 2017-12-26 |
WO2011024941A3 (ja) | 2011-04-28 |
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