JP2001073100A - Ferrous sintered compact, powder for manufacture of ferrous sintered compact, and manufacture of ferrous sintered compact - Google Patents
Ferrous sintered compact, powder for manufacture of ferrous sintered compact, and manufacture of ferrous sintered compactInfo
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- JP2001073100A JP2001073100A JP24614299A JP24614299A JP2001073100A JP 2001073100 A JP2001073100 A JP 2001073100A JP 24614299 A JP24614299 A JP 24614299A JP 24614299 A JP24614299 A JP 24614299A JP 2001073100 A JP2001073100 A JP 2001073100A
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- sintered body
- powder
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- 239000000843 powder Substances 0.000 title claims abstract description 109
- 238000004519 manufacturing process Methods 0.000 title claims description 17
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 title abstract 6
- 239000000463 material Substances 0.000 claims abstract description 42
- 239000000956 alloy Substances 0.000 claims abstract description 32
- 239000007787 solid Substances 0.000 claims abstract description 32
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 31
- 238000005245 sintering Methods 0.000 claims abstract description 30
- 239000000203 mixture Substances 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 19
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 17
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 15
- 230000001050 lubricating effect Effects 0.000 claims abstract description 13
- 229910052751 metal Inorganic materials 0.000 claims description 31
- 239000002184 metal Substances 0.000 claims description 30
- 239000002245 particle Substances 0.000 claims description 30
- 239000011159 matrix material Substances 0.000 claims description 26
- 239000000470 constituent Substances 0.000 claims description 22
- 239000000314 lubricant Substances 0.000 claims description 15
- 229910000905 alloy phase Inorganic materials 0.000 claims description 9
- 238000010791 quenching Methods 0.000 claims description 9
- 230000000171 quenching effect Effects 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 6
- 239000002861 polymer material Substances 0.000 claims description 5
- 239000007921 spray Substances 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010687 lubricating oil Substances 0.000 claims description 4
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 4
- 229910052582 BN Inorganic materials 0.000 claims description 3
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 229910044991 metal oxide Inorganic materials 0.000 claims description 3
- 150000004706 metal oxides Chemical class 0.000 claims description 3
- 239000010445 mica Substances 0.000 claims description 3
- 229910052618 mica group Inorganic materials 0.000 claims description 3
- 150000004767 nitrides Chemical class 0.000 claims description 3
- 230000006835 compression Effects 0.000 claims description 2
- 238000007906 compression Methods 0.000 claims description 2
- 238000005242 forging Methods 0.000 claims description 2
- 229910052976 metal sulfide Inorganic materials 0.000 claims description 2
- 239000004033 plastic Substances 0.000 claims description 2
- 238000005096 rolling process Methods 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 16
- 239000002244 precipitate Substances 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 abstract 1
- 150000003568 thioethers Chemical class 0.000 abstract 1
- 238000005461 lubrication Methods 0.000 description 21
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 19
- 230000000694 effects Effects 0.000 description 17
- 238000010438 heat treatment Methods 0.000 description 14
- 239000013078 crystal Substances 0.000 description 10
- 238000012360 testing method Methods 0.000 description 9
- 238000004453 electron probe microanalysis Methods 0.000 description 8
- 230000001965 increasing effect Effects 0.000 description 8
- 229910052742 iron Inorganic materials 0.000 description 7
- 238000001556 precipitation Methods 0.000 description 7
- 230000001771 impaired effect Effects 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 239000003921 oil Substances 0.000 description 6
- 238000009826 distribution Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000000523 sample Substances 0.000 description 5
- 150000004763 sulfides Chemical class 0.000 description 5
- 238000005299 abrasion Methods 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 229910052804 chromium Inorganic materials 0.000 description 4
- 230000006872 improvement Effects 0.000 description 4
- 229910052721 tungsten Inorganic materials 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 230000002411 adverse Effects 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 229910001566 austenite Inorganic materials 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 230000005496 eutectics Effects 0.000 description 3
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- 229910052748 manganese Inorganic materials 0.000 description 3
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- 229910052759 nickel Inorganic materials 0.000 description 3
- 238000000879 optical micrograph Methods 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
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- 229910052710 silicon Inorganic materials 0.000 description 3
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- 239000010959 steel Substances 0.000 description 3
- 229910052720 vanadium Inorganic materials 0.000 description 3
- 230000018199 S phase Effects 0.000 description 2
- 229910002056 binary alloy Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000002826 coolant Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000013011 mating Effects 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910001182 Mo alloy Inorganic materials 0.000 description 1
- 229910015325 MoFe Inorganic materials 0.000 description 1
- 108010038629 Molybdoferredoxin Proteins 0.000 description 1
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- 238000005275 alloying Methods 0.000 description 1
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
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- 238000005266 casting Methods 0.000 description 1
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- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
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- 238000007429 general method Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
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- 238000001513 hot isostatic pressing Methods 0.000 description 1
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- 230000006698 induction Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
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- 239000011347 resin Substances 0.000 description 1
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- 230000007480 spreading Effects 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000005211 surface analysis Methods 0.000 description 1
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- 238000005496 tempering Methods 0.000 description 1
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
Landscapes
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】この発明はＦｅ系焼結体、Ｆ
ｅ系焼結体製造用粉末、及びＦｅ系焼結体の製造方法に
関する。TECHNICAL FIELD The present invention relates to an Fe-based sintered body,
The present invention relates to a powder for producing an e-based sintered body and a method for producing an Fe-based sintered body.
【０００２】[0002]
【従来の技術及び発明が解決しようとする課題】各種機
械構造部品、とりわけ自動車部品において、その構成材
の摩擦係数を低減することはメカニックロス（機械損
失）を低減し、エネルギーの有効利用を図る上で有用で
ある。機械構造部品の摩擦係数を低減する手段として、
その構成材中にＭｏxＳy型の化合物を微細析出させ、そ
のＭｏxＳyの潤滑作用に基づいて摩擦係数を低減するこ
とが考えられる。2. Description of the Related Art Reducing the friction coefficient of the components of various mechanical structural parts, particularly automobile parts, reduces the mechanic loss (mechanical loss) and makes effective use of energy. Useful on As a means to reduce the coefficient of friction of mechanical structural parts,
It is conceivable that a MixSy-type compound is finely precipitated in the constituent material and the friction coefficient is reduced based on the lubricating action of the MixSy.
【０００３】従来Ｆｅ−Ｍｏ−Ｓ系の鋳造材においてこ
の種ＭｏxＳy型の化合物の析出が認められており、一部
では摩擦係数の低減が認められている（例えば、日本金
属学会誌３８（１９７４）２０６、２１３）。しかしな
がらかかる鋳造材の場合、図４（ａ）に示すように、同
時に、Ｆｅ系マトリックス相よりも融点の低いＦｅＳ相
１５１がネット状に形成され、そのネット状のＦｅＳ相
１５１が赤熱脆性の主原因となって、その後の熱間加工
を行うことができず、実際には工業的に利用されていな
いのが実情である。例えばＦｅ−Ｓ二元系状態図から推
測すれば、ＦｅＳ相とオーステナイト相とは共晶反応型
の疑似二元系を形成し、その共晶組成（Ｓが約３０重量
％）よりもＦｅリッチ側では融液を冷却するに伴い、ま
ずＦｅの初晶を生じ、その初晶の成長に伴い残液中には
Ｓ成分が濃化されてゆく。Ｓ成分は周知の通りＦｅ中で
は界面活性な元素であり、残液の固液境界付近に特に優
先的に集まりやすいと考えられる。そして、最終的に残
液は共晶温度にてオーステナイト相とＦｅＳ相とに共晶
分離するのであるが、残液は初晶結晶粒間の網目状空間
に押し込められる形となるので、形成されるＦｅＳ相も
ネット状になると考えることができる。いずれにしろ、
鋳造材の場合、凝固時におけるこのようなネット状のＦ
ｅＳ相が必ず生じ、その後の熱処理により過飽和のＳ成
分をマトリックス中に分散析出させてもネット状のＦｅ
Ｓ相は消滅せず、赤熱脆性の問題は避けがたいのであ
る。[0003] Conventionally, precipitation of this type of MoxSy type compound has been observed in Fe-Mo-S-based cast materials, and a reduction in the friction coefficient has been observed in some cases (for example, Journal of the Japan Institute of Metals 38 (1974)). ) 206, 213). However, in the case of such a cast material, as shown in FIG. 4 (a), at the same time, the FeS phase 151 having a lower melting point than the Fe-based matrix phase is formed in a net shape, and the net-shaped FeS phase 151 is mainly composed of red-hot embrittlement. As a cause, subsequent hot working cannot be performed, and the fact is that it is not actually used industrially. For example, when inferred from the Fe—S binary system phase diagram, the FeS phase and the austenite phase form a eutectic reaction type pseudo binary system, and the Fe-rich phase is more Fe-rich than its eutectic composition (S is about 30% by weight). On the side, primary crystals of Fe are generated as the melt is cooled, and the S component is concentrated in the remaining liquid as the primary crystals grow. As is well known, the S component is a surface-active element in Fe, and it is considered that it is likely to preferentially gather near the solid-liquid boundary of the residual liquid. Finally, the residual liquid is eutectic-separated into an austenite phase and an FeS phase at the eutectic temperature, but the residual liquid is formed because it is pressed into the network space between the primary crystal grains. The FeS phase can also be considered to be net-like. in any case,
In the case of a cast material, such a net-like F
An eS phase always occurs, and even if a supersaturated S component is dispersed and precipitated in the matrix by a subsequent heat treatment, a net-like Fe
The S phase does not disappear, and the problem of red embrittlement is inevitable.
【０００４】そこで、上記の問題を解決するために、特
開平１０−３１７００２号公報には、重量％で、Ｓ：１
〜１０％，Ｍｏ：３〜２５％で１．６７Ｓ＋１≦Ｍｏ≦
１．６７Ｓ＋７を満たし、残部不可避的不純物及びＦｅ
からなることを特徴とする低摩擦係数粉末を用いてＦｅ
系焼結体を製造する技術が開示されている。焼結材の場
合、ＦｅＳ相は融液の凝固反応が主体とならないので、
鋳造材のようなネット状形成は生じにくく、マトリック
ス中に分散形成され、結果として赤熱脆性が非常に生じ
にくくなる。これは、鋳造材と本質的に異なる点であ
る。[0004] In order to solve the above problem, Japanese Patent Application Laid-Open No. Hei 10-317002 discloses that S: 1
-10%, Mo: 1.67S + 1 ≦ Mo ≦ at 3-25%
1.67S + 7 is satisfied, the balance is inevitable impurities and Fe
Fe powder using a low coefficient of friction powder characterized by comprising
A technique for manufacturing a sintered body is disclosed. In the case of a sintered material, the FeS phase does not mainly involve the solidification reaction of the melt,
A net-like formation such as a cast material is unlikely to occur, and is dispersed and formed in a matrix. As a result, red-hot brittleness is extremely unlikely to occur. This is essentially different from the cast material.
【０００５】しかし、該公報に開示された組成範囲で
は、１．６７Ｓ＋１≦Ｍｏ≦１．６７Ｓ＋７の制約があ
るために、Ｍｏ含有量と連動してＳの含有量も増加せざ
るを得ない事情がある。例えばＳ含有量を最大に近い１
０重量％まで増加させたときに、許容されるＭｏの含有
量の上限は２４重量％程度である。そして、本発明者等
が鋭意検討した結果、Ｍｏに対するＳの相対含有量が増
え過ぎると、Ｓ成分は、ＦｅＳ等のＦｅ系硫化物（固体
潤滑効果をあまり期待できない）の生成に消費され、結
果として固体潤滑に効果的なＭｏxＳyを必要十分な量に
て形成できず、性能的に不十分なものしか得られないこ
とがわかった。However, in the composition range disclosed in the publication, there is a restriction of 1.67S + 1 ≦ Mo ≦ 1.67S + 7, so that the S content must be increased in conjunction with the Mo content. There is. For example, if the S content is
When it is increased to 0% by weight, the upper limit of the allowable Mo content is about 24% by weight. As a result of intensive studies by the present inventors, if the relative content of S with respect to Mo is excessively increased, the S component is consumed for generation of Fe-based sulfides such as FeS (solid lubricating effect is not expected much), As a result, it was found that a necessary and sufficient amount of MoxSy effective for solid lubrication could not be formed, and only those having insufficient performance could be obtained.
【０００６】本発明の課題は、ＭｏxＳy等、潤滑作用を
有するＳリッチ相を分散形成した組織が容易に得られ、
ひいては赤熱脆性を生じにくく、かつ均一で良好な潤滑
性能を達成することができるＦｅ系焼結体と、その製造
に使用する粉末、さらにはその粉末を用いたＦｅ系焼結
体の製造方法ならびに粉末の製造方法とを提供すること
にある。An object of the present invention is to easily obtain a structure in which an S-rich phase having a lubricating action such as MoxSy is dispersed and formed,
Further, an Fe-based sintered body that hardly causes red-hot brittleness and can achieve uniform and good lubricating performance, a powder used for the production thereof, and a method for producing an Fe-based sintered body using the powder, and And a method for producing a powder.
【０００７】[0007]
【課題を解決するための手段及び作用・効果】上記の課
題を解決するために、本発明のＦｅ系焼結体は、Ｆｅを
主成分とし、Ｓ成分を１〜４重量％、Ｍｏ成分を１８〜
３０重量％含有するとともに、Ｆｅを主成分とする金属
マトリックス相中に、平均的なＳ成分濃度が前記金属マ
トリックス相よりも高くなるＳリッチ相が分散形成され
ていることを特徴とする。なお、本明細書にて、「主成
分」（「主体」あるいは「主に」等も同義）とは、着目
している物質において、含有率の最も高い成分を意味す
る。なお、「成分」は、元素のほか、必要に応じ物質あ
るいは相を指すものとし、比率の単位は、「重量％」、
「体積％」、「面積比率％」など、個々に定めるものと
する。Means for Solving the Problems and Actions / Effects In order to solve the above-mentioned problems, the Fe-based sintered body of the present invention contains Fe as a main component, an S component of 1 to 4% by weight, and a Mo component. 18 ~
An S-rich phase having an average S component concentration higher than that of the metal matrix phase is dispersed and formed in a metal matrix phase containing 30% by weight and Fe as a main component. In this specification, “main component” (also synonymous with “subject” or “mainly”) means a component having the highest content of the substance of interest. The term “component” refers to a substance or a phase as necessary in addition to an element. The unit of the ratio is “% by weight”,
"Volume%", "area ratio%", etc. shall be determined individually.
【０００８】また、本発明のＦｅ系焼結体製造用粉末
は、Ｆｅを主成分とし、Ｓ成分を０．５〜４重量％、Ｍ
ｏ成分を１８〜３０重量％含有することを特徴とする。
この粉末を焼結することにより、上記本発明のＦｅ系焼
結体を製造することができる。The powder for producing an Fe-based sintered body of the present invention contains Fe as a main component, an S component of 0.5 to 4% by weight,
The o-component is characterized by containing 18 to 30% by weight.
By sintering this powder, the Fe-based sintered body of the present invention can be manufactured.
【０００９】なお、Ｓリッチ相は、例えば金属マトリッ
クス相中に分散析出した金属硫化物相を主体に形成され
るものである。The S-rich phase is formed mainly of, for example, a metal sulfide phase dispersed and precipitated in a metal matrix phase.
【００１０】Ｆｅを主成分とし、Ｓ成分を１〜４重量
％、Ｍｏ成分を１８〜３０重量％含有する焼結体製造用
粉末の焼結により、Ｆｅを主成分とする金属マトリック
ス相中に、Ｓリッチ相が分散形成された焼結体組織を容
易に得ることができる。すなわち、潤滑作用を有するＳ
リッチ相を分散形成したＦｅ系焼結体組織を実現するこ
とで、これを軸受けや機械摺動部品等に適用した場合
に、均一で良好な潤滑性能を達成することができる。ま
た、鋳造材におけるＦｅＳのようにＳリッチ相がネット
状（網状）に析出せず、分散形態で存在するので、焼結
体にさらに熱間加工を施したりする際に赤熱脆性の問題
も生じにくい。By sintering a powder for producing a sintered body containing Fe as a main component, S component at 1 to 4% by weight and Mo component at 18 to 30% by weight, a metal matrix phase containing Fe as a main component is obtained. And a sintered body structure in which the S-rich phase is dispersedly formed can be easily obtained. That is, S having lubricating action
By realizing the Fe-based sintered body structure in which the rich phase is dispersedly formed, when this is applied to a bearing, a mechanical sliding part, or the like, uniform and good lubrication performance can be achieved. Further, since the S-rich phase does not precipitate in the form of a net (like a net) like FeS in the cast material but exists in a dispersed form, there arises a problem of red hot brittleness when further performing hot working on the sintered body. Hateful.
【００１１】さらに、焼結体の組成を、Ｍｏ成分を１８
〜３０重量％に対し、Ｓ成分を１〜４重量％と、特開平
１０−３１７００２号公報に記載された発明よりＳ含有
量が相対的に低い組成を選択することにより、固体潤滑
性に優れたＭｏ系硫化物を主体とするＳリッチ相の形成
が促進され、良好な潤滑性能を有するＦｅ系焼結体が得
られるようになる。なお、参考のため、特開平１０−３
１７００２号公報のＭｏ及びＳの組成範囲ＰＡと、本発
明のＭｏ及びＳの組成範囲ＴＩとを図１に示している。Further, the composition of the sintered body was changed to 18
Excellent solid lubricity by selecting a composition in which the S component is relatively lower than that of the invention described in Japanese Patent Application Laid-Open No. 10-317002, with the S component being 1 to 4% by weight with respect to 30% by weight. The formation of an S-rich phase mainly composed of Mo-based sulfide is promoted, and an Fe-based sintered body having good lubrication performance can be obtained. For reference, see Japanese Patent Application Laid-Open No. 10-3
FIG. 1 shows the composition range PA of Mo and S in 17002 and the composition range TI of Mo and S of the present invention.
【００１２】Ｓ成分の含有量が１重量％未満であると、
後述のＭｏ系Ｓリッチ相あるいはＭｏ−Ｆｅ系Ｓリッチ
相の形成が不十分となり、焼結体の固体潤滑性能が損な
われることにつながる。他方、Ｓ成分が４重量％を超え
ると、ＦｅＳ等の固体潤滑に寄与しない硫化物生成が多
く生じ、焼結体の固体潤滑性能が同様に損なわれるほ
か、合金溶解時にＳ成分を均一に分布させることが困難
となる。なお、Ｓ成分の含有量はより望ましくは１〜３
重量％とするのがよい。When the content of the S component is less than 1% by weight,
The formation of the Mo-based S-rich phase or Mo-Fe-based S-rich phase described below becomes insufficient, leading to impaired solid lubrication performance of the sintered body. On the other hand, if the S component exceeds 4% by weight, a large amount of sulfides not contributing to solid lubrication such as FeS are generated, and the solid lubrication performance of the sintered body is similarly impaired, and the S component is uniformly distributed during melting of the alloy. It will be difficult to do so. The content of the S component is more desirably 1 to 3.
% By weight.
【００１３】他方、Ｍｏ成分が１８重量％未満になる
と、後述のＭｏ系Ｓリッチ相あるいはＭｏ−Ｆｅ系Ｓリ
ッチ相の形成が不十分となり、焼結体の固体潤滑性能が
損なわれることにつながる。他方、３０重量％以上Ｍｏ
を配合しても、硫化物相の形成量が飽和し、ひいては焼
結体の固体潤滑性能のそれ以上の向上が見込めなくなる
ため、高価なＭｏ成分が増える分だけコストアップを招
くことにつながる。さらに、Ｍｏ量が増加すると、焼結
温度によっては、焼結時の収縮量が大きくなり過ぎ、得
られる焼結部材の寸法精度の低下を来たしやすくなる。
なお、Ｍｏ成分の含有量はより望ましくは２０〜２８重
量％とするのがよい。On the other hand, if the Mo content is less than 18% by weight, the formation of the Mo-based S-rich phase or Mo-Fe-based S-rich phase described below becomes insufficient, and the solid lubrication performance of the sintered body is impaired. . On the other hand, 30% by weight or more of Mo
Even if it is blended, the formation amount of the sulfide phase is saturated, and further improvement in the solid lubrication performance of the sintered body cannot be expected. Therefore, the increase in the expensive Mo component leads to an increase in cost. Further, when the amount of Mo increases, the amount of shrinkage during sintering becomes too large depending on the sintering temperature, and the dimensional accuracy of the obtained sintered member tends to be reduced.
The content of the Mo component is more desirably 20 to 28% by weight.
【００１４】また、Ｍｏ含有量として、１８〜３０重量
％を採用することで、焼結体の収縮が促進され、その密
度及び強度を一層高めることが可能である。ただし、前
記した通り、Ｍｏ量が３０重量％を超えると収縮が進行
し過ぎ、また、焼結体の強度を担うＦｅ量が不足して、
却って強度低下を招くことがある。Further, by adopting the Mo content of 18 to 30% by weight, the shrinkage of the sintered body is promoted, and the density and strength thereof can be further increased. However, as described above, if the Mo amount exceeds 30% by weight, the shrinkage proceeds excessively, and the amount of Fe, which is responsible for the strength of the sintered body, is insufficient.
On the contrary, the strength may be reduced.
【００１５】なお、焼結体製造用粉末は、Ｆｅを主成分
とし、Ｓ成分を１〜４重量％、Ｍｏ成分を１８〜３０重
量％含有する組成となるように合金原料を溶解した後、
その原料を急冷する工程を経て製造された主要粉末を使
用することが望ましい。粉末製造に際して合金溶湯を急
冷することにより、鋳造材等におけるネット状のＦｅＳ
相形成が効果的に抑制され、図２に示すように、粉末粒
子６０’中においてＳリッチ相６０ｂが金属マトリック
ス相６０ａ中に分散した形態で析出させることができ
る。このような粉末は焼結後においても、図４（ｃ）に
示すように、例えば金属マトリックス結晶相粒子５１中
にＳリッチ相５２が分散した状態、あるいは図４（ｄ）
又は（ｅ）に示すように、金属マトリックス相結晶粒子
５１に対し、Ｓリッチ相結晶粒子５２が等軸晶的に分散
した状態（あるいは、（ｃ）と（ｄ）あるいは（ｅ）と
が混在した状態）となるなど、金属マトリックス相５１
中にＳリッチ相５２が分散した組織を維持しやすい。従
って、仮にＦｅＳが析出したとしても、粒界部等に偏在
した状態が形成されにくいので赤熱脆性が効果的に抑制
され、焼結体を加工する際にも容易にこれをなすことが
でき、目的とする形状を得ることができるのである。も
っとも粉末の場合、焼結に際して最終形状（ネットシェ
イプ）ないしこれに近い形状（ニアネットシェイプ）に
焼結することが可能であり、この場合には赤熱脆性自体
が問題とならない。The powder for producing a sintered body is prepared by dissolving an alloy material so as to have a composition containing Fe as a main component, an S component of 1 to 4% by weight, and a Mo component of 18 to 30% by weight.
It is desirable to use the main powder produced through the step of quenching the raw material. By quenching the molten alloy at the time of powder production, a net-like FeS
Phase formation is effectively suppressed, and as shown in FIG. 2, the S-rich phase 60b can be precipitated in the powder particles 60 ′ in a form dispersed in the metal matrix phase 60a. Even after sintering, such a powder is in a state in which the S-rich phase 52 is dispersed in the metal matrix crystal phase particles 51 as shown in FIG.
Or, as shown in (e), a state in which the S-rich phase crystal particles 52 are equiaxially dispersed in the metal matrix phase crystal particles 51 (or (c) and (d) or (e) are mixed) The metal matrix phase 51
It is easy to maintain a structure in which the S-rich phase 52 is dispersed. Therefore, even if FeS is precipitated, red-hot brittleness is effectively suppressed since a state unevenly distributed in a grain boundary portion or the like is not easily formed, and this can be easily performed even when processing a sintered body, The desired shape can be obtained. However, in the case of powder, it is possible to sinter to a final shape (net shape) or a shape close to this (near net shape) at the time of sintering, and in this case, red hot brittleness itself does not matter.
【００１６】また、さらに重要な点は、本発明に特有の
高Ｍｏの合金組成では、急冷法を採用することで、固体
潤滑に寄与しないＦｅＳの析出が抑制される一方、代わ
って固体潤滑に有効なＭｏ−Ｓ系あるいはＭｏ−Ｆｅ−
Ｓ系の硫化物の析出が促進され、一層潤滑性の良好な焼
結体の製造が可能となることである。これは、固溶限を
超えるＭｏの存在がＭｏ系硫化物の形成・析出を促すた
め、Ｆｅ系硫化物の形成に寄与するＳ成分が目減りして
Ｆｅ系硫化物の形での析出が抑制される、あるいはＦｅ
系硫化物がＭｏ系硫化物の成長のために分解されるため
であると推測される。More importantly, in the high Mo alloy composition peculiar to the present invention, by employing the quenching method, precipitation of FeS which does not contribute to solid lubrication is suppressed, while solid lubrication is used instead. Effective Mo-S system or Mo-Fe-
Precipitation of S-based sulfide is promoted, and the production of a sintered body having better lubricity becomes possible. This is because the presence of Mo exceeding the solid solubility limit promotes the formation and precipitation of Mo-based sulfides, so the S component contributing to the formation of Fe-based sulfides is reduced, and the precipitation in the form of Fe-based sulfides is suppressed. Or Fe
This is presumed to be because the system sulfide is decomposed due to the growth of the Mo system sulfide.
【００１７】具体的には、急冷工程は、図２に示すよう
に、合金溶湯７１を液体冷却媒及び／又は気体冷却媒７
９とともに噴霧する噴霧工程を採用できる。例えば、同
軸的に配置された内ノズル７８と外ノズル７７からなる
噴霧ノズルに対し、内ノズル７８内に合金溶湯７１を供
給し、先端側の開口部７１ａから流出させながら、両ノ
ズル７８，７７間の隙間７９を経て不活性ガスあるいは
水等の噴霧媒体を開口部７７ａから噴射することによ
り、合金溶湯を噴霧・凝固させる。これにより得られる
噴霧粉末粒子６０’は粒径が概ね１０〜３００μｍ程度
であるが、さらに細かい粉末が必要な場合は、図２
（ｃ）に示すように、さらに粉砕（あるいは分級）して
二次粉末６１’となすこともできる。なお、噴霧法以外
では合金電極を消耗電極として高速回転させ、陰極（例
えばタングステン系金属製のもの）からのアークにより
部分溶解して飛散させる回転電極法を採用することもで
きる。さらに、ロール急冷法、スプラット急冷法等によ
り合金溶湯をリボン状あるいはフレーク状に凝固させ、
これを粉砕して粉末化する方法も可能である。Specifically, in the quenching step, as shown in FIG. 2, the molten alloy 71 is cooled by a liquid cooling medium and / or a gas cooling medium 7.
A spraying step of spraying with 9 can be adopted. For example, the alloy melt 71 is supplied into the inner nozzle 78 to the spray nozzle composed of the inner nozzle 78 and the outer nozzle 77 which are coaxially arranged, and flows out from the opening 71a on the distal end side while the two nozzles 78, 77 are being discharged. The molten alloy is sprayed and solidified by injecting a spray medium such as an inert gas or water from the opening 77a through the gap 79 between them. The sprayed powder particles 60 'thus obtained have a particle size of about 10 to 300 μm, but if a finer powder is required, FIG.
As shown in (c), it can be further pulverized (or classified) to form the secondary powder 61 '. In addition to the spraying method, a rotating electrode method in which an alloy electrode is rotated at high speed as a consumable electrode and partially melted and scattered by an arc from a cathode (for example, a tungsten-based metal) may be employed. Further, the alloy melt is solidified into a ribbon or flake by a roll quenching method, a splat quenching method, or the like.
It is also possible to pulverize and pulverize this.
【００１８】焼結体組織中におけるＳリッチ相は、Ｍｏ
及びＳの含有量が、それらの組織全体の平均的な含有量
よりも大きくなるＭｏ系Ｓリッチ相と、Ｍｏ及びＳの含
有量が、それらの組織全体の平均的な含有量よりも大き
くなり、かつＦｅを含有するのＭｏ−Ｆｅ系Ｓリッチ相
との、少なくともいずれかを主体とするものとなる。前
者は例えばＭｏxＳy型のＭｏ硫化物相であり、焼結体組
織表面における成分濃度分析を電子プローブ微小解析
（ＥＰＭＡ）により行ったときに、Ｍｏの特性Ｘ線とＳ
の特性Ｘ線とが同時に観測されるとともに、観測される
特性Ｘ線はこれら両元素からのものが主となる領域であ
る。一方、後者は、焼結体組織表面における成分濃度分
析をＥＰＭＡにより同様に行ったときに、Ｍｏの特性Ｘ
線とＳの特性Ｘ線のほかＦｅの特性Ｘ線が、前記したＭ
ｏ系Ｓリッチ相よりも高いレベルにて同時に観測される
領域である。これは、ＭｏxＳy型硫化物相あるいはＦｅ
xＳy型硫化物相にＦｅあるいはＭｏが固溶したものであ
るか、あるいはＥＰＭＡ等では識別が困難な２μｍ以下
の微細な結晶形態にて、ＭｏxＳy型硫化物相とＦｅxＳy
型硫化物相とが混在したもの、あるいはそれら両者のい
ずれとも異なるＭｏ−Ｆｅ系複合硫化物のいずれかであ
ると推測される。なお、Ｍｏ系Ｓリッチ相及びＭｏ−Ｆ
ｅ系Ｓリッチ相はいずれも、これらの固体潤滑性能が著
しく損なわれない範囲にて、他の合金元素あるいは不可
避不純物が含有されていてもよい。The S-rich phase in the structure of the sintered body is Mo
And the S-rich phase in which the contents of S and S are larger than the average content of the entire structure, and the contents of Mo and S are higher than the average content of the entire structure. And at least one of a Mo-Fe-based S-rich phase containing Fe. The former is, for example, a MoSy type Mo sulfide phase. When the component concentration analysis on the surface of the sintered body structure is performed by electron probe microanalysis (EPMA), the characteristic X-rays of Mo and S
Characteristic X-rays are simultaneously observed, and the observed characteristic X-rays are regions mainly from these two elements. On the other hand, in the latter, when the component concentration analysis on the surface of the sintered body structure was similarly performed by EPMA, the characteristic X
The characteristic X-ray of Fe in addition to the characteristic X-ray of
This is a region that is simultaneously observed at a higher level than the o-based S-rich phase. This is due to the fact that the MoxSy type sulfide phase or Fe
Fe or Mo is dissolved in xSy-type sulfide phase, or it is difficult to distinguish by EPMA or the like.
It is presumed to be either a mixture of the sulfide type and the Mo-Fe-based composite sulfide different from both of them. The Mo-based S-rich phase and Mo-F
Any of the e-based S-rich phases may contain other alloying elements or unavoidable impurities as long as the solid lubrication performance is not significantly impaired.
【００１９】なお、Ｍｏ系Ｓリッチ相及びＭｏ−Ｆｅ系
Ｓリッチ相の焼結体組織中の面積比率は、焼結体の表面
を研磨してＥＰＭＡの面分析を行い、Ｍｏ、Ｆｅ及びＳ
の特性Ｘ線強度（これは各成分の濃度を反映した指標で
ある）の分布をマッピングするとともに、そのマッピン
グ結果を合成することによりＭｏ系Ｓリッチ相領域とＭ
ｏ−Ｆｅ系Ｓリッチ相領域とを画像的に識別して、各々
面積計算することにより求めることができる。なお、Ｓ
リッチ相は、組織全体の平均的なＳ濃度レベルよりもＳ
濃度の高い領域として定め、Ｍｏ系Ｓリッチ相及びＭｏ
−Ｆｅ系Ｓリッチ相は、Ｆｅ濃度、Ｍｏ濃度及びＳ濃度
が、それぞれ組織全体の平均的Ｆｅ濃度、Ｍｏ濃度及び
Ｓ濃度レベルよりも高い領域として識別可能である。な
お、組織全体の平均的なＭｏ濃度及びＳ濃度レベルより
もＭｏ濃度及びＳ濃度が高くなる領域において、その平
均的なＦｅ濃度よりもＦｅ濃度が高いか否かにより、Ｍ
ｏ−Ｆｅ系Ｓリッチ相及びＭｏ系Ｓリッチ相を互いに識
別することができる。The area ratio of the Mo-based S-rich phase and the Mo-Fe-based S-rich phase in the structure of the sintered body was determined by polishing the surface of the sintered body and analyzing the surface of EPMA to determine the Mo, Fe and S contents.
The distribution of the characteristic X-ray intensity (this is an index reflecting the concentration of each component) is mapped, and the mapping result is synthesized to obtain the Mo-based S-rich phase region and M
The o-Fe-based S-rich phase region can be image-wise identified and calculated by calculating the area of each. Note that S
The rich phase has a higher S concentration than the average S concentration level in the whole tissue.
Defined as a region with high concentration, Mo-based S-rich phase and Mo-based
The Fe-based S-rich phase can be identified as a region where the Fe concentration, the Mo concentration, and the S concentration are higher than the average Fe concentration, the Mo concentration, and the S concentration level of the entire tissue, respectively. Note that, in a region where the Mo concentration and the S concentration are higher than the average Mo concentration and the S concentration level of the entire tissue, M is determined depending on whether the Fe concentration is higher than the average Fe concentration.
The o-Fe-based S-rich phase and the Mo-based S-rich phase can be distinguished from each other.
【００２０】いずれにせよ、Ｓリッチ相は、これらＭｏ
系Ｓリッチ相とＭｏ−Ｆｅ系Ｓリッチ相とが主体となる
場合に、良好な固体潤滑性能を有するＦｅ系焼結体が実
現されるのである。具体的には、焼結体組織の断面にて
観察されるＭｏ系Ｓリッチ相とＭｏ−Ｆｅ系Ｓリッチ相
との合計の面積比率が１２％〜５０％となっているのが
よい。該面積比率が１２％未満では、焼結体の固体潤滑
性能が損なわれることにつながる。他方、Ｍｏ系Ｓリッ
チ相とＭｏ−Ｆｅ系Ｓリッチ相との合計が４０％以上に
なると、焼結体の強度あるいは靭性が却って損なわれる
場合がある。上記の面積比率は、望ましくは１２〜４０
％となっているのがよい。In any case, the S-rich phase is composed of these Mo
When the system-S rich phase and the Mo-Fe-based S-rich phase are mainly used, an Fe-based sintered body having good solid lubrication performance is realized. Specifically, the total area ratio of the Mo-based S-rich phase and the Mo-Fe-based S-rich phase observed in the cross section of the sintered body structure is preferably 12% to 50%. If the area ratio is less than 12%, the solid lubrication performance of the sintered body will be impaired. On the other hand, if the total of the Mo-based S-rich phase and the Mo-Fe-based S-rich phase is 40% or more, the strength or toughness of the sintered body may be impaired. The area ratio is desirably 12 to 40.
It is better to be%.
【００２１】一方、焼結体の固体潤滑性能をさらに良好
なものとするには、Ｍｏ−Ｆｅ系Ｓリッチ相が形成され
ていることが望ましく、焼結体組織に占めるＭｏ−Ｆｅ
系Ｓリッチ相の面積比率を特に２％〜２０％となすこと
が、上記の観点において特に望ましい。On the other hand, in order to further improve the solid lubrication performance of the sintered body, it is desirable that a Mo-Fe-based S-rich phase is formed, and that the Mo-Fe
It is particularly desirable from the above viewpoint that the area ratio of the system S-rich phase is particularly 2% to 20%.
【００２２】次に、本発明の粉末を用いてＦｅ系焼結合
金を製造することの利点は、焼結条件や焼結後の熱処理
条件を変更することにより、析出するＳリッチ相の量
や、金属マトリックス相あるいはＳリッチ相の結晶粒径
分布など、その組織を目的に応じて自由に設定できる点
である。例えば、図４（ｃ）は、比較的低温にて焼結を
行っうか、あるいは焼結時に蒸発あるいは分解してキャ
ビティを形成する高分子材料フィラーを配合して焼結を
行った場合で、組織中にはキャビティが残留し、焼結体
の密度も低くなる。ただし、これが連通気孔である場合
には、ここに潤滑油や潤滑高分子材料を含浸すること
で、一層潤滑性能に優れた部材を得ることができる。こ
の場合、図３に示すように粉末６０を、プレス等により
成型体６１となし、その成形体６１を焼結して焼結体６
２とする一般的な方法のほか、空隙率を高めるために、
セラミックコンテナ等に充填するのみで、特に圧縮成型
せずに焼結を行うこともできる。なお、潤滑高分子材料
として、例えばポリ四フッ化エチレン（ＰＴＦＥ、商品
名：テフロン）等のフッ素樹脂を例示することができる
が、これに限られるものではない。Next, the advantage of producing an Fe-based sintered alloy using the powder of the present invention is that the amount of the precipitated S-rich phase can be reduced by changing the sintering conditions and the heat treatment conditions after sintering. In addition, the structure such as the crystal grain size distribution of the metal matrix phase or the S-rich phase can be freely set according to the purpose. For example, FIG. 4C shows a case where sintering is performed at a relatively low temperature or a polymer material filler that evaporates or decomposes at the time of sintering to form a cavity is mixed and sintered. Cavities remain therein, and the density of the sintered body decreases. However, when this is a continuous ventilation hole, a member having more excellent lubrication performance can be obtained by impregnating it with a lubricating oil or a lubricating polymer material. In this case, as shown in FIG. 3, the powder 60 is formed into a molded body 61 by pressing or the like, and the molded body 61 is sintered to form a sintered body 6.
In addition to the general method of 2, to increase the porosity,
Sintering can also be performed by merely filling a ceramic container or the like without performing compression molding. In addition, as the lubricating polymer material, for example, a fluororesin such as polytetrafluoroethylene (PTFE, trade name: Teflon) can be exemplified, but it is not limited thereto.
【００２３】焼結温度が低い場合（例えば１０００〜１
１５０℃）は、図２（ｂ）において粉末粒子中６０’中
に析出しているＳリッチ相６０ｂが、図４（ｃ）に示す
ように、比較的微細なまま焼結後の組織にも引き継がれ
る場合がある。その後、比較的低温にて熱処理を行えば
（例えば８００〜１０００℃）、微細析出したＳリッチ
相５２の量をさらに増やすことも可能である。他方、焼
結温度を比較的高く設定した場合（例えば１１５０〜１
３００℃）、あるいは焼結後に熱処理を施した場合（例
えば８００〜１０００℃）は、図４（ｄ）及び（ｅ）に
示すように、元のＳリッチ相から周辺にＳ成分が拡散し
て拡がり、Ｓリッチ相の量（面積比率あるいは体積比
率）を多くすることができる。When the sintering temperature is low (for example, 1000 to 1)
(150 ° C.) indicates that the S-rich phase 60b precipitated in the powder particles 60 ′ in FIG. 2 (b) has a relatively fine structure after sintering as shown in FIG. 4 (c). May be taken over. Thereafter, if heat treatment is performed at a relatively low temperature (for example, 800 to 1000 ° C.), the amount of the finely precipitated S-rich phase 52 can be further increased. On the other hand, when the sintering temperature is set relatively high (for example, 1150 to 1
When the heat treatment is performed after sintering (for example, 800 to 1000 ° C.), as shown in FIGS. 4D and 4E, the S component diffuses from the original S-rich phase to the periphery. Spreading can increase the amount (area ratio or volume ratio) of the S-rich phase.
【００２４】なお、焼結方法は、常圧焼結法のほか、高
密度化が必要な場合は、ホットプレス法や熱間等方圧プ
レス（ＨＩＰ）の採用も可能である。また、Ｆｅ系焼結
体製造用粉末を一次圧縮及び一次焼結処理した後、再圧
縮及び再焼結処理して最終の焼結体を得るようにするこ
とも、焼結体の高密度化を図る上で有効である。このよ
うにした場合、比摩耗量をより効果的に少なくできるこ
とが確認されている。尚本発明の粉末は、これを用いて
溶射による被覆やＰＰＷ（プラズマパウダー溶接）等の
肉盛溶接を行うことも可能である。他方、Ｆｅ系焼結体
製造用粉末を、ビレット等の一次素材形状に成形及び焼
結した後、その一次素材に鍛造、圧延等の塑性加工を施
すことにより線材、棒材及び板材等の二次素材形状を得
る方法も可能である。後者の場合、本発明の採用により
焼結後の熱間加工時の赤熱脆性が回避できる利点がある
ことは、既に説明した通りである。As the sintering method, in addition to the normal pressure sintering method, when high density is required, a hot press method or a hot isostatic pressing (HIP) can be adopted. In addition, after the powder for producing an Fe-based sintered body is subjected to primary compression and primary sintering, recompression and resintering is performed to obtain a final sintered body. It is effective in aiming at. In this case, it has been confirmed that the specific wear amount can be reduced more effectively. The powder of the present invention can be used for coating by thermal spraying or overlay welding such as PPW (plasma powder welding). On the other hand, after forming and sintering the powder for producing an Fe-based sintered body into a primary material shape such as a billet, the primary material is subjected to plastic working such as forging or rolling to obtain a secondary material such as a wire, a rod and a plate. A method of obtaining the next material shape is also possible. In the latter case, as described above, there is an advantage that adoption of the present invention can avoid red hot brittleness during hot working after sintering.
【００２５】なお、Ｓリッチ相の分散性を高めて固体潤
滑性能を均一で良好なものとする観点においては、Ｓリ
ッチ相の平均粒径を０．５〜５０μｍ程度とすることが
望ましい。なお、本明細書にてＳリッチ相の平均粒径と
は、焼結体組織表面にてＳリッチ相の結晶粒がエッチン
グ等により明確に観察できる場合は、その組織写真上に
多数の測定ラインを引き、各結晶粒領域が切り取る測定
ラインの長さの平均値にて表すものとする（いわゆるラ
インインターセプト法）。他方、走査型電子顕微鏡（Ｓ
ＥＭ）に組み込まれたＥＰＭＡを用いて面分析を行い、
そのマッピング結果から画像化されるＳリッチ相領域
に、ＳＥＭ写真から求められる結晶粒界位置を重ね合わ
せ、同様にラインインターセプタ法を用いて測定する方
法もある。From the viewpoint of enhancing the dispersibility of the S-rich phase to make the solid lubrication performance uniform and good, it is desirable that the average particle size of the S-rich phase is about 0.5 to 50 μm. In the present specification, the average particle size of the S-rich phase is defined as the number of measurement lines on the structure photograph when crystal grains of the S-rich phase can be clearly observed on the surface of the sintered structure by etching or the like. , And expressed as an average value of the length of the measurement line cut out by each crystal grain region (so-called line intercept method). On the other hand, a scanning electron microscope (S
Surface analysis is performed using EPMA incorporated in EM),
There is also a method in which a crystal grain boundary position obtained from an SEM photograph is superimposed on an S-rich phase region imaged from the mapping result, and measurement is similarly performed using a line interceptor method.
【００２６】また、潤滑油等の含浸を行う場合は別とし
て、焼結体に一層十分な強度を付与したい場合には、焼
結体の密度を５．５ｇ／ｃｍ３以上としておくことが望
ましい。Apart from the case where lubricating oil or the like is impregnated, when it is desired to impart more sufficient strength to the sintered body, it is desirable to set the density of the sintered body to 5.5 g / cm 3 or more. .
【００２７】本発明に従って粉末製造し、焼結すること
によって機械構造部品等を製造する場合、低摩擦係数特
性を更に高めたり或いは他の特性を容易に付与できる利
点が得られる。即ち、先ず粉末製造してその焼結により
機械構造部品等を製造する場合、粉末ないし粉末焼結の
利点を最大限に利用して粉末に黒鉛等のＣの粉末を添加
混合し、以て焼結体中に炭化物形成及び母相の硬さを向
上させることができる。In the case of producing mechanical structural parts by producing and sintering powder according to the present invention, there is obtained an advantage that the low friction coefficient characteristic can be further enhanced or other characteristics can be easily imparted. That is, in the case of first producing powder and sintering to produce mechanical structural parts, etc., the powder or C powder such as graphite is added to and mixed with the powder by making the most of the advantages of the powder or powder sintering. It is possible to improve the formation of carbides and the hardness of the matrix in the binder.
【００２８】本発明においては、粉末ひいてはそれによ
って製造される焼結体に、Ｃ（Ｃ粉末の形で添加できる
ことを既に説明した）、Ｓｉ、Ｍｎ、Ｖ、Ｗ、Ｎｉ及び
Ｃｒの１種又は２種以上を含有させることができる。そ
れらの望ましい含有範囲と、その理由について以下に詳
述する。 (1)Ｃ：０．０５〜１．２重量％ Ｃは強度を確保するのに有用な元素である。但し０．０
５％未満では効果が乏しく、逆に過剰添加はＭｏ炭化物
の析出を過度に促進し、Ｍｏ硫化物の形成に悪影響を与
えるため上限を１．２％とする。 (2)Ｓｉ：≦２．０重量％ Ｓｉは溶鋼中の酸素低減に有効で湯流れを改善し、焼結
体の生地を強化する元素である。２．０％でその効果が
飽和するのでこれを上限とする。なお、一定の効果を期
待する場合は、０．１重量％以上は含有されていること
が望ましい。In the present invention, one kind of C (as already described that it can be added in the form of C powder), Si, Mn, V, W, Ni and Cr is added to the powder and the sintered body produced therefrom. Two or more can be contained. The desirable content ranges and the reasons are described in detail below. (1) C: 0.05 to 1.2% by weight C is an element useful for securing strength. However 0.0
If it is less than 5%, the effect is poor. Conversely, excessive addition excessively promotes the precipitation of Mo carbide and adversely affects the formation of Mo sulfide, so the upper limit is made 1.2%. (2) Si: ≦ 2.0% by weight Si is an element that is effective in reducing oxygen in molten steel, improves the flow of molten metal, and strengthens the material of the sintered body. Since the effect is saturated at 2.0%, the upper limit is set. When a certain effect is expected, it is desirable that the content is 0.1% by weight or more.
【００２９】(3)Ｍｎ：≦２．０重量％ Ｍｎは鋼の焼入れ性を確保するのに有効な元素である
が、過度の添加は粉末の酸化を促進するため上限を２．
０重量％とする。なお、一定の効果を期待する場合は、
０．０５重量％以上は含有されていることが望ましい。 (4)Ｎｉ：≦５．０重量％ Ｎｉは焼入れ性を与え、焼入れ・焼戻し後の機械的性質
を向上させる。但し過度の添加は残留オーステナイト生
成の原因となり、硬さを低下させるので上限を５．０重
量％とする。なお、一定の効果を期待する場合は、０．
５重量％以上は含有されていることが望ましい。 (5)Ｃｒ：≦１．５０重量％ Ｃｒは鋼の焼入れ性を確保するのに有効であるが、過度
の添加はＭｏと副炭化物を作り、Ｍｏ硫化物の生成に悪
影響を与えるので上限を１．５０重量％とする。なお、
一定の効果を期待する場合は、０．３重量％以上は含有
されていることが望ましい。(3) Mn: ≦ 2.0% by weight Mn is an effective element for securing the hardenability of steel, but excessive addition promotes oxidation of the powder.
0% by weight. If you expect a certain effect,
It is desirable that the content be 0.05% by weight or more. (4) Ni: ≦ 5.0% by weight Ni gives quenchability and improves mechanical properties after quenching and tempering. However, excessive addition causes generation of residual austenite and lowers the hardness, so the upper limit is made 5.0 wt%. In addition, when a certain effect is expected, 0.
It is desirable to contain 5% by weight or more. (5) Cr: ≦ 1.50 wt% Cr is effective for securing the hardenability of steel, but excessive addition forms Mo and a sub-carbide and adversely affects the formation of Mo sulfide. 1.50% by weight. In addition,
When a certain effect is expected, it is desirable to contain 0.3% by weight or more.
【００３０】(6)Ｖ：≦３．０重量％ Ｖは単独でＶＣを形成し、耐摩耗性を与えるのに有効で
ある。但し過度の添加は粉末製造時の注湯ノズル閉塞等
のトラブルの要因となるので上限を３．０重量％とす
る。なお、一定の効果を期待する場合は、０．３重量％
以上は含有されていることが望ましい。 (7)Ｗ：≦１．０重量％ Ｗは炭化物を形成して耐摩耗性を与えるのに有効であ
る。但し過度の添加はＭｏと副炭化物を作り、Ｍｏ硫化
物の生成に悪影響を与えるので上限を１．０重量％とす
る。なお、一定の効果を期待する場合は、０．１重量％
以上は含有されていることが望ましい。(6) V: ≦ 3.0% by weight V alone forms VC and is effective in giving abrasion resistance. However, excessive addition may cause troubles such as clogging of a pouring nozzle during powder production, so the upper limit is set to 3.0% by weight. If a certain effect is expected, 0.3% by weight
It is desirable that the above be contained. (7) W: ≦ 1.0% by weight W is effective for forming carbides to give abrasion resistance. However, excessive addition produces Mo and secondary carbides and adversely affects the formation of Mo sulfide, so the upper limit is made 1.0% by weight. If a certain effect is expected, 0.1% by weight
It is desirable that the above be contained.
【００３１】例えば、焼結体（あるいは、後述の主要組
織構成相）の具体的な組成として、Ｃ、Ｓｉ、Ｍｎ、
Ｖ、Ｗ、Ｎｉ及びＣｒの１種又は２種以上を上記の範囲
にて含有し、残部Ｆｅと不可避不純物とからなる組成を
例示できる。For example, specific compositions of a sintered body (or a main structural constituent phase described later) include C, Si, Mn,
One or more of V, W, Ni and Cr are contained in the above range, and a composition comprising the balance of Fe and unavoidable impurities can be exemplified.
【００３２】次に、本発明においては、Ｆｅを主成分と
し、Ｓ成分を０．５〜４重量％、Ｍｏ成分を１８〜３０
重量％含有する上記の合金粉末を主要粉末として、その
主要粉末に、その主要粉末とは異なる材質にて構成され
る補助粉末を２〜４１体積％の範囲内にて配合すること
も可能である。得られる焼結体は、Ｆｅを主成分とし、
Ｓ成分を１〜４重量％、Ｍｏ成分を１８〜３０重量％含
有するとともに、Ｆｅを主成分とする金属マトリックス
相中に、平均的なＳ成分濃度が金属マトリックス相より
も高くなるＳリッチ相が分散形成された組織を主要組織
構成相として、その主要組織構成相とは異なる材質にて
構成される補助組織構成相を、焼結体組織の断面にて観
察される面積率にて７〜５５％の範囲内にて含有するも
のとなる。補助粉末の配合により、主要組織構成相の特
性に補助組織構成相に基づく種々の特性を付加すること
ができ、材料の応用範囲をさらに広げることができる。Next, in the present invention, Fe is the main component, the S component is 0.5-4% by weight, and the Mo component is 18-30%.
It is also possible to mix the above-mentioned alloy powder containing 10% by weight as a main powder with an auxiliary powder composed of a material different from that of the main powder within a range of 2 to 41% by volume. . The obtained sintered body has Fe as a main component,
An S-rich phase containing 1 to 4% by weight of the S component and 18 to 30% by weight of the Mo component and having an average S component concentration higher than that of the metal matrix phase in the metal matrix phase mainly containing Fe. Is defined as a main structural constituent phase, and an auxiliary structural constituent phase made of a material different from that of the main structural constituent phase is formed at an area ratio of 7 to 7 observed at a cross section of the sintered body structure. It will be contained within the range of 55%. By blending the auxiliary powder, various characteristics based on the auxiliary structural constituent phase can be added to the characteristics of the main structural constituent phase, and the application range of the material can be further expanded.
【００３３】なお、ＳおよびＭｏの必須添加元素成分
と、及びＣ、Ｓｉ、Ｍｎ、Ｖ、Ｗ、Ｎｉ及びＣｒ等の任
意添加元素成分の焼結体あるいは粉末中の望ましい含有
範囲、さらには焼結体中の各種Ｓリッチ相の望ましい含
有範囲は既に説明した通りであるが、補助粉末の配合に
伴い焼結体中に補助組織構成相が形成される場合は、上
記添加元素成分の粉末中あるいは焼結体中の望ましい含
有範囲、さらには焼結体中のＳリッチ相の望ましい含有
範囲は、各々、主要粉末中あるいは主要組織構成相中の
含有範囲として成立していることが望ましい。なお、補
助粉末が、上記の必須添加元素成分あるいは任意添加元
素成分を含有する結果、補助粉末に含有されるそれら成
分が、主要組織構成相（すなわち、Ｆｅ系マトリックス
相＋Ｓリッチ相）の形成に関与する場合があり、他方、
Ｃの配合により金属炭化物が形成される場合は、その炭
化物は補助組織構成相に属するものと考える。The desirable content range of the essential additive element components of S and Mo and the optional additive component components such as C, Si, Mn, V, W, Ni and Cr in the sintered body or powder, and further, The desirable content range of the various S-rich phases in the sintered body is as described above. However, when the auxiliary structural constituent phase is formed in the sintered body with the blending of the auxiliary powder, the content of the above-mentioned additional element component powder Alternatively, the desirable content range in the sintered body and the desirable content range of the S-rich phase in the sintered body are desirably established as the content range in the main powder or the main structural constituent phase, respectively. In addition, as a result of the auxiliary powder containing the above-mentioned essential additive element component or optional additive element component, those components contained in the auxiliary powder are converted into a main structural constituent phase (that is, Fe-based matrix phase + S-rich phase). May be involved,
When a metal carbide is formed by the blending of C, the carbide is considered to belong to the auxiliary structural constituent phase.
【００３４】補助粉末は、例えば、Ａｌ系合金粉末、Ｃ
ｕ系合金粉末及びＦｅ系合金粉末の少なくともいずれか
を主体とするものを採用できる。これに対応して補助組
織構成相も、Ａｌ系合金相及びＣｕ系合金相の少なくと
もいずれかを主体とするものとすることができる（Ｆｅ
系合金粉末は、Ｆｅ系マトリックス相の形成に主に寄与
する）。Ａｌ系合金相からなる補助組織構成相は、焼結
材料の軽量化と伝熱性向上等に寄与する。Ｃｕ系合金相
からなる補助組織構成相は、Ａｌ系合金相以上に焼結材
料の伝熱性向上に寄与する。なお、Ａｌ系合金粉末及び
Ｃｕ系合金粉末は、主要粉末に対する配合量によっては
押出成形による連続製造も可能となり、生産性向上にも
寄与する。他方、Ｆｅ系合金粉末は、例えばステンレス
鋼や系耐熱合金等で構成することができる。これによ
り、焼結部材の耐食性や耐熱性の向上を図ることが可能
となる。なお、補助組織構成相をなすＡｌ系合金相ある
いはＣｕ系合金相は、固体潤滑相として機能する場合が
ある。また、以下に説明する固体潤滑剤粒子相や無機耐
摩耗粒子相も、補助組織構成相の一種であり、その形成
に使用する固体潤滑剤粉末及び無機耐摩耗粒子は補助粉
末の一種である。The auxiliary powder is, for example, Al alloy powder, C
A powder mainly composed of at least one of a u-based alloy powder and an Fe-based alloy powder can be employed. Correspondingly, the auxiliary structure constituent phase can be mainly composed of at least one of the Al-based alloy phase and the Cu-based alloy phase (Fe
The alloy powder mainly contributes to the formation of the Fe matrix phase. The auxiliary structural constituent phase composed of the Al-based alloy phase contributes to the reduction of the weight of the sintered material and the improvement of the heat conductivity. The auxiliary structure constituent phase composed of the Cu-based alloy phase contributes to the improvement of the heat conductivity of the sintered material more than the Al-based alloy phase. The Al-based alloy powder and the Cu-based alloy powder can be continuously manufactured by extrusion molding depending on the compounding amount with respect to the main powder, which contributes to an improvement in productivity. On the other hand, the Fe-based alloy powder can be made of, for example, stainless steel or a heat-resistant alloy. This makes it possible to improve the corrosion resistance and heat resistance of the sintered member. Note that the Al-based alloy phase or Cu-based alloy phase serving as an auxiliary structure constituent phase may function as a solid lubricating phase. The solid lubricant particle phase and the inorganic wear-resistant particle phase described below are also a kind of auxiliary structure constituent phase, and the solid lubricant powder and the inorganic wear-resistant particles used for the formation thereof are a kind of auxiliary powder.
【００３５】すなわち、窒化硼素、二硫化モリブデン、
雲母、黒鉛等の固体潤滑剤粉末を所定量添加することに
よって、焼結体の摩擦係数を更に一段と低減することが
容易に実現できる。他方、焼結温度を低く設定すること
により、固体潤滑剤粉末としてフッ素樹脂（例えば、ポ
リテトラフルオロエチレンなど）の粉末を採用すること
も可能である（なお、前記した連通気孔に含浸されるフ
ッ素樹脂は当然に補助組織構成相とみなす）。固体潤滑
剤粒子は、粉末中に２〜４１体積％の範囲内にて含有さ
せることにより、焼結体中にも同様の割合で含有させる
ことができる。２体積％未満では潤滑性向上効果が顕著
でなく、４１体積％を超えると混合が難しいため、分布
が偏在化して焼結体の強度低下を来す場合がある。な
お、体積含有率は、組織中に占める面積比率とも対応
し、該面積比率の範囲は７〜５５％とすることが望まし
い。なお、二硫化モリブデンを固体潤滑剤粉末として使
用した焼結体では、二硫化モリブデン粉末粒子はＭｏ系
Ｓリッチ相の形成に与る形となる。That is, boron nitride, molybdenum disulfide,
By adding a predetermined amount of solid lubricant powder such as mica, graphite, etc., it is possible to easily further reduce the friction coefficient of the sintered body. On the other hand, by setting the sintering temperature low, it is also possible to employ a powder of a fluororesin (for example, polytetrafluoroethylene) as the solid lubricant powder (the fluorine impregnated in the above-mentioned interconnected pores). The resin is of course considered the constituent phase of the auxiliary tissue). By including the solid lubricant particles in the powder in the range of 2 to 41% by volume, the same ratio can be contained in the sintered body. If it is less than 2% by volume, the effect of improving lubricity is not remarkable, and if it exceeds 41% by volume, mixing is difficult, so that the distribution may be unevenly distributed and the strength of the sintered body may be reduced. The volume content corresponds to the area ratio in the tissue, and the range of the area ratio is desirably 7 to 55%. In a sintered body using molybdenum disulfide as the solid lubricant powder, the molybdenum disulfide powder particles take a form that contributes to the formation of the Mo-based S-rich phase.
【００３６】一方、金属炭化物、金属窒化物、金属炭窒
化物及び金属酸化物の少なくともいずれかを主体とする
無機耐摩耗粒子を所定量、例えば２〜４１体積％の範囲
内にて添加することによって、焼結体の耐摩耗性を効果
的に高めることが容易に実現できる。２体積％未満では
耐摩耗性向上効果が顕著でなく、４１体積％を超えると
混合が難しいため、分布が偏在化して焼結体の強度低下
を来す場合がある。なお、この場合も体積含有率は、組
織中に占める面積比率とも対応し、該面積比率の範囲は
７〜５５％とすることが望ましい。On the other hand, inorganic wear-resistant particles mainly composed of at least one of a metal carbide, a metal nitride, a metal carbonitride and a metal oxide are added in a predetermined amount, for example, in the range of 2 to 41% by volume. Accordingly, it is possible to easily increase the wear resistance of the sintered body effectively. If it is less than 2% by volume, the effect of improving the wear resistance is not remarkable, and if it exceeds 41% by volume, mixing is difficult, so that the distribution may be unevenly distributed and the strength of the sintered body may be reduced. In this case, the volume content also corresponds to the area ratio in the tissue, and the range of the area ratio is desirably 7 to 55%.
【００３７】本発明においては固体潤滑剤粉末及び無機
耐摩耗粒子の２種類以上のものを複合で添加混合するこ
とももちろん可能である。この場合において固体潤滑剤
粉末、無機耐摩耗粒子の添加量はそれぞれ上記範囲と
し、かつそれらの合計量で添加量が４１体積％以下とす
るのがよい。また、固体潤滑剤粉末及び／又は無機耐摩
耗粒子と、前記のＣの粉末とを複合で添加混合すること
も可能である。In the present invention, it is of course possible to add and mix two or more solid lubricant powders and inorganic wear-resistant particles in a composite form. In this case, the addition amounts of the solid lubricant powder and the inorganic wear-resistant particles are preferably in the above ranges, and the total amount thereof is preferably 41% by volume or less. It is also possible to add and mix the solid lubricant powder and / or the inorganic wear-resistant particles and the powder of C in a composite manner.
【００３８】[0038]
【実験例】以下、本発明の効果を確認するために以下の
実験を行った。まず、３０ｋｇ誘導炉にて合金原料を溶
解し、これを水噴霧装置にて噴霧することにより、表１
に示す各種組成の合金粉末を主要粉末として製造した。EXPERIMENTAL EXAMPLES The following experiments were conducted to confirm the effects of the present invention. First, the alloy raw material was melted in a 30 kg induction furnace, and sprayed with a water spray device, thereby obtaining Table 1.
Alloy powders of various compositions shown in Table 1 were produced as main powders.
【００３９】[0039]
【表１】 [Table 1]
【００４０】得られた粉末は乾燥後、６０メッシュ以下
に分級するとともに、還元性の雰囲気中で焼鈍を施した
後、試験に供した。そして、該焼鈍後の粉末に潤滑剤と
してステアリン酸亜鉛を０．５重量％添加・混合して原
料粉末とした。なお、番号１３〜２２については、上記
の合金粉末（主要粉末）に対し、補助粉末として固体潤
滑材粉末粒子あるいは無機耐摩耗粒子を各種体積含有率
にて配合した。原料粉末は、金型を用いて７ｔ／ｃｍ２
の圧力で成形し、その圧粉体を１２００℃で１ｈｒ、水
素ガス中で焼結した。なお、成型体の寸法は１０ｍｍ×
１０ｍｍ×５０ｍｍの直方体状であり、焼結体としたと
きの寸法変化から収縮率を算出した。その結果、Ｍｏ量
が３０重量％未満の焼結体では収縮率は１０％以下であ
ったのに対し、３０重量％を超える番号５の試料では１
２％と大きくなっていた。焼結体は、８００〜１０００
℃にて２時間、真空中で熱処理（焼鈍）し、さらに切削
及び砥石研磨加工により、表面粗さ２μｍＲａ程度の粗
さとなるように仕上げた。また比較のために鋳造材と市
販のＳ４５Ｃ材を用い、削り出しによって同形状の試験
片を得た。The obtained powder was dried, classified to 60 mesh or less, annealed in a reducing atmosphere, and then subjected to a test. Then, 0.5% by weight of zinc stearate as a lubricant was added to and mixed with the annealed powder to obtain a raw material powder. In addition, with respect to Nos. 13 to 22, solid lubricant powder particles or inorganic wear-resistant particles were mixed at various volume contents as auxiliary powders with the above-mentioned alloy powder (main powder). The raw material powder is 7 t / cm 2 using a mold.
The compact was sintered at 1200 ° C. for 1 hour in hydrogen gas. The size of the molded body is 10 mm x
The shrinkage ratio was calculated from the dimensional change when the sintered body was a rectangular parallelepiped of 10 mm x 50 mm. As a result, the shrinkage rate was 10% or less for the sintered body having the Mo amount of less than 30% by weight, whereas the shrinkage rate was 1% for the sample of No.
It was 2%. The sintered body is 800 to 1000
Heat treatment (annealing) was performed at a temperature of 2 ° C. for 2 hours in a vacuum, followed by cutting and grinding with a grindstone to finish to a surface roughness of about 2 μmRa. For comparison, a cast material and a commercially available S45C material were used, and a test piece having the same shape was obtained by cutting.
【００４１】番号１〜４の組成については焼結後、１０
００℃にて２時間熱処理したものについて、表面をバフ
研磨し、ナイタールにてエッチング後、組織の光学顕微
鏡写真を倍率４００倍にて撮影した。結果を図５〜図８
に示す（番号１〜４にそれぞれ対応）。写真中、白く表
れているのがＦｅあるいはＭｏを主体とする金属マトリ
ックス相であり、黒あるいは濃いグレーにて表れている
のが硫化物相（Ｓリッチ相）である。いずれも硫化物相
が組織中に分散形成されていることがわかるが、Ｍｏ含
有量の少ない番号１（図５）の組織では、硫化物相の量
がやや少なくなっている。また、Ｍｏ含有量が比較的多
い番号３、４（図７，８）では、硫化物相が非常に細か
く分散形成されていることがわかる。After sintering, the compositions of Nos. 1 to 4
After heat treatment at 00 ° C. for 2 hours, the surface was buffed and etched with nital, and an optical microscope photograph of the structure was taken at 400 × magnification. The results are shown in FIGS.
(Corresponding to numbers 1 to 4, respectively). In the photograph, white is the metal matrix phase mainly composed of Fe or Mo, and black or dark gray is the sulfide phase (S-rich phase). In each case, it is found that the sulfide phase is dispersed and formed in the structure. However, in the structure of No. 1 (FIG. 5) having a small Mo content, the amount of the sulfide phase is slightly reduced. In addition, it can be seen that the sulfide phases are very finely dispersed and formed in Nos. 3 and 4 (FIGS. 7 and 8) in which the Mo content is relatively large.
【００４２】また、同じ番号１〜４の組成について、熱
処理前後に焼結体組織表面における成分濃度分析を電子
プローブ微小解析（ＥＰＭＡ）により行い、Ｍｏ−Ｆｅ
系Ｓリッチ相（略号：ＭｏＦｅＳ、Ｍｏ含有量：３０重
量％以上、Ｆｅ含有量：４５重量％以上、Ｓ含有量：
３．０重量％以上）、Ｆｅ系Ｓリッチ相（略号：Ｆｅ
Ｓ、Ｆｅ含有量：４５重量％以上、Ｓ含有量：３．０重
量％以上）、Ｍｏ系Ｓリッチ相（略号：ＭｏＳ、Ｍｏ含
有量：３０重量％以上、Ｓ含有量：３．０重量％以
上）、Ｍｏ−Ｆｅ系マトリックス相（略号：ＭｏＦｅ、
Ｍｏ含有量：３０重量％以上、Ｆｅ含有量：４５重量％
以上）、遊離Ｓ相（略号：Ｓ、Ｓが３重量％以上）、Ｆ
ｅ系相（略号：Ｆｅ、Ｆｅが４５重量％以上）、Ｍｏ系
相（略号：Ｍｏ、Ｍｏが３０重量％以上）を、その元素
分布マッピングから識別してそれぞれの面積率を求め
た。結果を表２及び図９に示す。なお、各写真からライ
ンインターセプト法により求めた硫化物相の平均粒径
は、番号１が約１０μｍ、番号２が約３μｍ、番号３が
約２μｍ、番号４が約１．６μｍであった。With respect to the same compositions of Nos. 1 to 4, component concentration analysis on the surface of the sintered body structure was performed by electron probe microanalysis (EPMA) before and after the heat treatment.
S-rich phase (abbreviation: MoFeS, Mo content: 30% by weight or more, Fe content: 45% by weight or more, S content:
3.0 wt% or more), Fe-based S-rich phase (abbreviation: Fe
S, Fe content: 45% by weight or more, S content: 3.0% by weight or more, Mo-based S-rich phase (abbreviation: MoS, Mo content: 30% by weight or more, S content: 3.0% by weight) %), A Mo—Fe-based matrix phase (abbreviation: MoFe,
Mo content: 30% by weight or more, Fe content: 45% by weight
Above), free S phase (abbreviation: S, S is 3% by weight or more), F
The e-phase (abbreviation: Fe, Fe is 45% by weight or more) and the Mo-based phase (abbreviation: Mo, Mo is 30% by weight or more) were identified from their element distribution mappings, and the respective area ratios were determined. The results are shown in Table 2 and FIG. The average particle size of the sulfide phase obtained from each photograph by the line intercept method was about 10 μm for No. 1, about 3 μm for No. 2, about 2 μm for No. 3, and about 1.6 μm for No. 4.
【００４３】[0043]
【表２】 [Table 2]
【００４４】Ｍｏ量が増加するに従い、Ｍｏ−Ｆｅ系Ｓ
リッチ相及びＭｏ系Ｓリッチ相の面積率が増大している
ことがわかる。また、熱処理によりＭｏ−Ｆｅ系Ｓリッ
チ相及びＭｏ系Ｓリッチ相（特に前者）の成長がさらに
促進される一方、Ｆｅ系Ｓリッチ相の量は逆に減少して
いることもわかる。なお、Ｍｏ−Ｆｅ系マトリックス相
は、Ｆｅ２ＭｏあるいはＦｅ３Ｍｏ等の金属化合物を主
体に構成されていると考えられる。これらの金属関化合
物相は焼結材料の耐摩耗性を向上させる効果を有してい
る。As the amount of Mo increases, the Mo—Fe based S
It can be seen that the area ratios of the rich phase and the Mo-based S-rich phase are increasing. It can also be seen that the heat treatment further promotes the growth of the Mo-Fe-based S-rich phase and the Mo-based S-rich phase (particularly the former), while the amount of the Fe-based S-rich phase is reduced. It is considered that the Mo—Fe-based matrix phase mainly includes a metal compound such as Fe 2 Mo or Fe 3 Mo. These metal-related compound phases have an effect of improving the wear resistance of the sintered material.
【００４５】次に、番号１〜４の組成について、熱処理
前後の硬度及び密度レベルを、ロックウェルＢスケール
硬度計（圧子：１．６ｍｍ球状、荷重１００ｋｇｆ）に
て測定した。硬度の測定結果を表３及び図１０に示す。Next, for the compositions of Nos. 1 to 4, the hardness and density level before and after the heat treatment were measured with a Rockwell B scale hardness meter (indenter: 1.6 mm spherical, load: 100 kgf). The measurement results of the hardness are shown in Table 3 and FIG.
【００４６】[0046]
【表３】 [Table 3]
【００４７】この結果によると、８００℃熱処理では硬
度が上昇し、９００℃ないし１０００℃熱処理では、硬
度が逆に減少している。これは、８００℃（範囲では、
７５０〜８５０℃）熱処理では、マトリックス相中に過
飽和固溶していたＳ成分がＳリッチ相として微細に析出
するため、その析出強化効果により硬度が上昇したもの
と考えられる。他方、９００℃以上ではＳリッチ相がオ
ストワルト成長し、却って硬度が低下したものと考えら
れる。一方、いずれの熱処理条件においても、Ｍｏの含
有量が２２〜２９重量％において、硬度が顕著に増大し
ていることがわかる。According to the results, the hardness increases with the heat treatment at 800 ° C., and decreases with the heat treatment at 900 ° C. to 1000 ° C. This is 800 ° C (in the range,
In the heat treatment at 750 to 850 ° C., the supersaturated S component in the matrix phase is finely precipitated as an S-rich phase, and it is considered that the hardness is increased due to the precipitation strengthening effect. On the other hand, at 900 ° C. or higher, it is considered that the S-rich phase grew Ostwald and the hardness was rather lowered. On the other hand, under any of the heat treatment conditions, it can be seen that the hardness is significantly increased when the Mo content is 22 to 29% by weight.
【００４８】また、密度の結果を表４及び図１１に示
す。熱処理品については、熱処理温度が９００℃と１０
００℃とで密度がわずかに低下している。これについて
は、前述のオストワルト成長に起因するものと考えられ
る。The results of the density are shown in Table 4 and FIG. For heat-treated products, the heat treatment temperature is 900 ° C and 10 ° C.
The density slightly decreased at 00 ° C. This is considered to be due to the Ostwald growth described above.
【００４９】[0049]
【表４】 [Table 4]
【００５０】次に、摩擦係数及び摩耗量の測定を以下の
ようにして行った。まず、本発明材として、組成は表５
に示すものにて焼結後、１０００℃で２時間熱処理した
試験片を用意した。なお、比較のために、同一成分の鋳
造材と市販の炭素鋼（Ｓ４５Ｃ）とを用い、削り出しに
よって同形状の試験片も合わせて作成した）。そして定
荷重、往復運動下における摩擦係数測定を無潤滑と油塗
布（油含浸）の条件下で測定した。ここで荷重は１０ｋ
ｇ／ｍｍ２，摩擦係数測定は１００往復後の安定した時
点で行った。また油含浸材については、焼結体の空孔の
効果を確認するために室温と３００℃の２つの温度条件
下で測定を行った。結果を表５に示す。Next, the measurement of the coefficient of friction and the amount of wear were performed as follows. First, the composition of the material of the present invention is shown in Table 5
And then heat-treated at 1000 ° C. for 2 hours to prepare test pieces. Note that, for comparison, a test piece having the same shape was also prepared by cutting out a cast material having the same component and a commercially available carbon steel (S45C). Then, the coefficient of friction under a constant load and reciprocating motion was measured under conditions of no lubrication and oil application (oil impregnation). Here the load is 10k
g / mm 2 , the coefficient of friction was measured at a stable point after 100 reciprocations. Further, the oil impregnated material was measured under two temperature conditions of room temperature and 300 ° C. in order to confirm the effect of pores in the sintered body. Table 5 shows the results.
【００５１】[0051]
【表５】 [Table 5]
【００５２】この結果から、本発明材は比較材（Ｓ４５
Ｃ）よりも摩擦係数が低くなっていることがわかる。ま
た同一成分の鋳造材と本発明材とは、無潤滑下ではほぼ
同じ摩擦係数であるものの、油を含浸させた条件下では
その含油効果により、本発明材が鋳造材に比べて摩擦係
数が小さく、特に３００℃の下では鋳造材に比べて本発
明材の方が著しく含油効果が高いことが分かる。From the results, the material of the present invention was compared with the comparative material (S45).
It can be seen that the coefficient of friction is lower than that of C). Although the cast material of the same component and the material of the present invention have almost the same friction coefficient under no lubrication, the oil of the present invention has a coefficient of friction that is lower than that of the cast material due to its oil impregnating effect under oil impregnated conditions. It can be seen that the material of the present invention is remarkably higher in oil-impregnating effect at 300 ° C., especially at 300 ° C. than the cast material.
【００５３】次に、表１の番号１〜２２の全組成におい
て焼結後、１０００℃で２時間熱処理した各種試験片を
用意し、摩擦係数の測定と耐摩耗性の評価を次の条件で
行った。すなわち、摩擦係数の測定は定荷重、往復運動
下における摩擦係数を無潤滑で測定することにより行っ
た。このときの荷重は１０ｋｇ／ｍｍ２であり、また摩
擦係数は１００往復後の安定した時点で測定した。さら
に、耐摩耗性評価は、相手材ＳＫＤ１１（焼入れ焼き戻
し材：ロックウェルＣスケール硬度ＨRC＝５８）、荷重
２ｋｇ、摩擦距離１００ｍ、無潤滑の条件で大越式摩耗
試験により行った。ここで比摩耗量とは、相手材ＳＫＤ
１１から成る直径３０ｍｍφ，厚みｔ＝３ｍｍの円盤を
供試材に荷重２ｋｇで押し付けた状態で円盤を回転さ
せ、供試材表面に生じた窪みの大きさ（面積）を表わし
たものである。結果を表１に示す。本発明に属する焼結
体として構成した試験片では、摩擦係数及び摩耗量のい
ずれも小さく、良好な潤滑性能が得られていることがわ
かる。Next, after sintering all the compositions of Nos. 1 to 22 in Table 1, various test pieces were prepared which were heat-treated at 1000 ° C. for 2 hours, and the friction coefficient was measured and the wear resistance was evaluated under the following conditions. went. That is, the coefficient of friction was measured by measuring the coefficient of friction under constant load and reciprocating motion without lubrication. The load at this time was 10 kg / mm 2 , and the coefficient of friction was measured at a stable point after 100 reciprocations. Further, the abrasion resistance was evaluated by the Ogoshi type abrasion test under the conditions of a mating material SKD11 (hardened and tempered material: Rockwell C scale hardness HRC = 58), a load of 2 kg, a friction distance of 100 m, and no lubrication. Here, the specific wear amount is defined as the mating material SKD
11 shows the size (area) of a depression formed on the surface of a test material by rotating the disk in a state where a disk made of No. 11 having a diameter of 30 mmφ and a thickness t = 3 mm is pressed against the test material under a load of 2 kg. Table 1 shows the results. In the test piece constituted as a sintered body belonging to the present invention, both the coefficient of friction and the amount of wear are small, and it can be seen that good lubrication performance is obtained.
【図１】本発明のＦｅ系焼結合金の組成範囲を示す図。FIG. 1 is a view showing a composition range of an Fe-based sintered alloy of the present invention.
【図２】噴霧法により急冷粉末を製造する方法を模式的
に示す図。FIG. 2 is a view schematically showing a method for producing a quenched powder by a spray method.
【図３】粉末を焼結して焼結体を製造する様子を示す
図。FIG. 3 is a view showing a state in which powder is sintered to produce a sintered body.
【図４】焼結合金の組織を鋳造剤の組織と対比させて示
す模式図。FIG. 4 is a schematic diagram showing the structure of a sintered alloy in comparison with the structure of a casting agent.
【図５】実験例の番号１の組成の焼結体試料の組織を示
す光学顕微鏡写真。FIG. 5 is an optical micrograph showing the structure of a sintered body sample having a composition of No. 1 in an experimental example.
【図６】同じく番号２の組成の焼結体試料の組織を示す
光学顕微鏡写真。FIG. 6 is an optical micrograph showing the structure of a sintered body sample having the composition of No. 2;
【図７】同じく番号３の組成の焼結体試料の組織を示す
光学顕微鏡写真。FIG. 7 is an optical microscope photograph showing the structure of a sintered body sample having the composition of No. 3;
【図８】同じく番号４の組成の焼結体試料の組織を示す
光学顕微鏡写真。FIG. 8 is an optical micrograph showing the structure of a sintered body sample having the composition of No. 4;
【図９】硫化物の面積率の測定結果を示すグラフ。FIG. 9 is a graph showing the measurement results of the area ratio of sulfide.
【図１０】焼結体中のＭｏ含有量と硬度測定結果を示す
グラフ。FIG. 10 is a graph showing the Mo content in a sintered body and the results of hardness measurement.
【図１１】焼結体中のＭｏ含有量と密度測定結果を示す
グラフ。FIG. 11 is a graph showing Mo content and density measurement results in a sintered body.
６０’，６１’ Ｆｅ系焼結体製造用粉末 ６２ Ｆｅ系焼結体 60 ', 61' Powder for producing Fe-based sintered body 62 Fe-based sintered body
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｃ２２Ｃ 33/02 Ｃ２２Ｃ 33/02 Ｂ １０３ １０３Ａ Ｆターム(参考） 4K017 AA04 BA06 BB04 BB15 EK01 4K018 AA24 AB01 AB02 AB03 AB04 AB05 AB07 AB10 AC01 BA02 BA08 BA16 EA51 FA01 FA47 KA02 ──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. 7 Identification symbol FI theme coat ゛ (reference) C22C 33/02 C22C 33/02 B 103 103A F term (reference) 4K017 AA04 BA06 BB04 BB15 EK01 4K018 AA24 AB01 AB02 AB03 AB04 AB05 AB07 AB10 AC01 BA02 BA08 BA16 EA51 FA01 FA47 KA02
Claims (30)
％、Ｍｏ成分を１８〜３０重量％含有するとともに、Ｆ
ｅを主成分とする金属マトリックス相中に、平均的なＳ
成分濃度が前記金属マトリックス相よりも高くなるＳリ
ッチ相が分散形成されていることを特徴とするＦｅ系焼
結体。1. An alloy containing Fe as a main component, an S component in an amount of 1 to 4% by weight, a Mo component in an amount of 18 to 30% by weight, and an F component.
In the metal matrix phase containing e as the main component, the average S
An Fe-based sintered body, wherein an S-rich phase having a component concentration higher than that of the metal matrix phase is dispersed and formed.
％、Ｍｏ成分を１８〜３０重量％含有するとともに、Ｆ
ｅを主成分とする金属マトリックス相中に、平均的なＳ
成分濃度が前記金属マトリックス相よりも高くなるＳリ
ッチ相が分散形成された組織を主要組織構成相として、
その主要組織構成相とは異なる材料系にて構成される補
助組織構成相を、焼結体組織の断面にて観察される面積
率にて７〜５５％の範囲内にて含有することを特徴とす
るＦｅ系焼結体。2. An alloy containing Fe as a main component, an S component in an amount of 1 to 4% by weight, a Mo component in an amount of 18 to 30% by weight, and an F component.
In the metal matrix phase containing e as the main component, the average S
The structure in which the S-rich phase in which the component concentration is higher than the metal matrix phase is dispersedly formed is defined as a main structural constituent phase,
It is characterized by containing an auxiliary structure constituent phase composed of a material system different from the main structure constituent phase within a range of 7 to 55% in an area ratio observed in a cross section of the sintered body structure. Fe-based sintered body.
ス相中に分散析出した金属硫化物相を主体に形成される
請求項１又は２に記載のＦｅ系焼結体。3. The Fe-based sintered body according to claim 1, wherein the S-rich phase is formed mainly of a metal sulfide phase dispersed and precipitated in the metal matrix phase.
が、それらの組織全体の平均的な含有量よりも大きくな
るＭｏ系Ｓリッチ相と、Ｍｏ及びＳの含有量が、それら
の組織全体の平均的な含有量よりも大きくなり、かつＦ
ｅを含有するのＭｏ−Ｆｅ系Ｓリッチ相との、少なくと
もいずれかを主体とするものである請求項３記載のＦｅ
系焼結体。4. The S-rich phase has a Mo-based S-rich phase in which the contents of Mo and S are larger than the average content of the whole structure thereof, and a content of Mo and S in which the contents of Mo and S are Greater than the average content of the whole tissue and F
4. The Fe according to claim 3, which is mainly composed of at least one of a Mo-Fe-based S-rich phase containing e.
Series sintered body.
Ｓリッチ相とＭｏ−Ｆｅ系Ｓリッチ相との合計の面積比
率が１２％〜４０％である請求項４記載のＦｅ系焼結
体。5. The Fe-based alloy according to claim 4, wherein the total area ratio of the Mo-based S-rich phase and the Mo—Fe-based S-rich phase observed in the cross section of the sintered body structure is 12% to 40%. Sintered body.
Ｆｅ系Ｓリッチ相の面積比率が２％〜２０％である請求
項４又は５に記載のＦｅ系焼結体。6. Mo- observed in a cross section of a sintered body structure.
The Fe-based sintered body according to claim 4 or 5, wherein an area ratio of the Fe-based S-rich phase is 2% to 20%.
リッチ相の平均粒径が０．５〜５０μｍである請求項１
ないし６のいずれかに記載のＦｅ系焼結体。7. The method according to claim 1, wherein said S is observed in a cross section of a sintered body structure.
The average particle size of the rich phase is 0.5 to 50 µm.
7. The Fe-based sintered body according to any one of items 1 to 6.
る請求項１ないし７のいずれかに記載のＦｅ系焼結体。8. The Fe-based sintered body according to claim 1, wherein the C content is 0.05 to 1.2% by weight.
Ｍｎと、３．０重量以下のＶと、１重量％以下のＷと、
５．０重量％以下のＮｉと、１．５０重量％以下のＣｒ
との１種又は２種以上を含有する請求項１ないし８のい
ずれかに記載のＦｅ系焼結体。9. up to 2% by weight of Si, up to 2% by weight of Mn, up to 3.0% by weight of V, up to 1% by weight of W;
5.0% by weight or less of Ni and 1.50% by weight or less of Cr
The Fe-based sintered body according to any one of claims 1 to 8, comprising at least one of the following.
ッチ相とは異なる組成を有する固体潤滑剤粒子相を、焼
結体組織の断面にて観察される面積率にて７〜５５％の
範囲内で含有する請求項２ないし９のいずれかに記載の
Ｆｅ系焼結体。10. A solid lubricant particle phase having a composition different from that of the S-rich phase as the auxiliary structure constituent phase in a range of 7 to 55% in area ratio observed in a cross section of the sintered body structure. The Fe-based sintered body according to any one of claims 2 to 9, wherein the sintered body is contained.
雲母、黒鉛及びフッ素樹脂の少なくともいずれかを主体
とするものである請求項１０記載のＦｅ系焼結体。11. The solid lubricant particle phase comprises boron nitride,
The Fe-based sintered body according to claim 10, which is mainly composed of at least one of mica, graphite, and a fluororesin.
耗粒子相を、焼結体組織の断面にて観察される面積率に
て７〜５５％の範囲内にて含有する請求項２ないし１１
のいずれかに記載のＦｅ系焼結体。12. The inorganic wear-resistant particle phase as the auxiliary structure constituting phase is contained within a range of 7 to 55% in terms of an area ratio observed in a cross section of the sintered body structure.
The Fe-based sintered body according to any one of the above.
物、金属窒化物、金属炭窒化物及び金属酸化物の少なく
ともいずれかを主体とするものである請求項１２記載の
Ｆｅ系焼結体。13. The Fe-based sintered body according to claim 12, wherein the inorganic wear-resistant particle phase is mainly composed of at least one of a metal carbide, a metal nitride, a metal carbonitride, and a metal oxide.
及びＣｕ系合金相の少なくともいずれかを主体とするも
のである請求項２ないし１３のいずれかに記載のＦｅ系
焼結体。14. The Fe-based sintered body according to claim 2, wherein the auxiliary structure constituent phase is mainly composed of at least one of an Al-based alloy phase and a Cu-based alloy phase.
又は潤滑高分子材料を含浸した請求項１ないし１４のい
ずれかに記載のＦｅ系焼結体。15. The Fe-based sintered body according to claim 1, wherein a continuous vent formed in the sintered body is impregnated with a lubricating oil or a lubricating polymer material.
４重量％、Ｍｏ成分を１８〜３０重量％含有することを
特徴とするＦｅ系焼結体製造用粉末。16. An alloy containing Fe as a main component and an S component of 0.5 to
A powder for producing an Fe-based sintered body, comprising 4% by weight and 18 to 30% by weight of a Mo component.
４重量％、Ｍｏ成分を１８〜３０重量％含有する主要粉
末に、その主要粉末とは異なる材質の補助粉末を２〜４
１体積％の範囲内にて配合したことを特徴とするＦｅ系
焼結体製造用粉末。17. An alloy containing Fe as a main component and an S component of 0.5 to
A main powder containing 4% by weight and an Mo component of 18 to 30% by weight, and an auxiliary powder having a material different from that of the main powder in 2-4%
A powder for producing an Fe-based sintered body, wherein the powder is blended within a range of 1% by volume.
である請求項１６又は１７に記載のＦｅ系焼結体製造用
粉末。18. The C content is 0.05 to 1.2% by weight.
The powder for producing an Fe-based sintered body according to claim 16 or 17, wherein
のＭｎと、３．０重量以下のＶと、１重量％以下のＷ
と、５．０重量％以下のＮｉと、１．５０重量％以下の
Ｃｒとの１種又は２種以上を含有する請求項１６ないし
１８のいずれかに記載のＦｅ系焼結体製造用粉末。19. up to 2% by weight of Si, up to 2% by weight of Mn, up to 3.0% of V and up to 1% by weight of W
19. The powder for producing an Fe-based sintered body according to claim 16, wherein the powder contains one or more of Ni, 5.0% by weight or less, and Cr, 1.50% by weight or less. .
を２〜４１体積％の範囲内にて含有する請求項１７ない
し１９のいずれかに記載のＦｅ系焼結体製造用粉末。20. The powder for producing an Fe-based sintered body according to claim 17, further comprising solid lubricant particles as the auxiliary powder in a range of 2 to 41% by volume.
硫化モリブデン、雲母、黒鉛及びフッ素樹脂の少なくと
もいずれかを主体とするものである請求項２０記載のＦ
ｅ系焼結体製造用粉末。21. The F according to claim 20, wherein the solid lubricant particles are mainly composed of at least one of boron nitride, molybdenum disulfide, mica, graphite and fluororesin.
Powder for manufacturing e-based sintered bodies.
を２〜４１体積％の範囲内にて含有する請求項１７ない
し２１のいずれかに記載のＦｅ系焼結体製造用粉末。22. The powder for producing an Fe-based sintered body according to claim 17, wherein said auxiliary powder contains inorganic wear-resistant particles in a range of 2 to 41% by volume.
金属窒化物、金属炭窒化物及び金属酸化物の少なくとも
いずれかを主体とするものである請求項２２記載のＦｅ
系焼結体製造用粉末。23. The inorganic wear-resistant particles are metal carbide,
23. The Fe according to claim 22, which is mainly composed of at least one of a metal nitride, a metal carbonitride and a metal oxide.
Powder for manufacturing sintered compacts.
ｕ系合金粉末及びＦｅ系合金粉末の少なくともいずれか
を主体とするものである請求項２３記載のＦｅ系焼結体
製造用粉末。24. The auxiliary powder comprises an Al-based alloy powder,
24. The powder for producing an Fe-based sintered body according to claim 23, wherein the powder mainly comprises at least one of a u-based alloy powder and an Fe-based alloy powder.
のＦｅ系焼結体の製造方法であって、請求項１６ないし
２４のいずれかに記載のＦｅ系焼結体製造用粉末を焼結
する工程を含むことを特徴とするＦｅ系焼結体の製造方
法。25. The method for producing an Fe-based sintered body according to any one of claims 1 to 15, wherein the powder for producing an Fe-based sintered body according to any one of claims 16 to 24 is sintered. A method for producing a Fe-based sintered body, comprising:
縮及び一次焼結処理した後、再圧縮及び再焼結処理して
最終の焼結体を得る請求項２５記載のＦｅ系焼結体の製
造方法。26. The Fe-based sintering according to claim 25, wherein the powder for producing an Fe-based sintered body is subjected to primary compression and primary sintering, followed by recompression and resintering to obtain a final sintered body. How to make the body.
ット等の一次素材形状に成形及び焼結した後、その一次
素材に鍛造、圧延等の塑性加工を施すことにより線材、
棒材及び板材等の二次素材形状を得る請求項２５又は２
６に記載の焼結体の製造方法。27. After forming and sintering the powder for producing an Fe-based sintered body into a primary material such as a billet, the primary material is subjected to plastic working such as forging or rolling to obtain a wire rod.
26. A secondary material shape such as a bar or a plate is obtained.
7. The method for producing a sintered body according to item 6.
体として製造し、その連通気孔に潤滑油又は潤滑高分子
材料を含浸させる請求項２７記載のＦｅ系焼結体の製造
方法。28. The method according to claim 27, wherein the sintered body is manufactured as a porous body having continuous vents, and the continuous vents are impregnated with a lubricating oil or a lubricating polymer material.
量％、Ｍｏ成分を１８〜３０重量％含有する組成となる
ように合金原料を溶解した後、その原料を急冷する工程
を含むことを特徴とするＦｅ系焼結体製造用粉末の製造
方法。29. A method comprising the steps of: melting an alloy raw material so as to have a composition containing Fe as a main component, an S component of 1 to 4% by weight, and a Mo component of 18 to 30% by weight, and quenching the raw material. A method for producing a powder for producing an Fe-based sintered body, characterized in that:
求項２９記載にＦｅ系焼結体製造用粉末の製造方法。30. The method according to claim 29, wherein the quenching step includes a spray quenching step.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24614299A JP2001073100A (en) | 1999-08-31 | 1999-08-31 | Ferrous sintered compact, powder for manufacture of ferrous sintered compact, and manufacture of ferrous sintered compact |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24614299A JP2001073100A (en) | 1999-08-31 | 1999-08-31 | Ferrous sintered compact, powder for manufacture of ferrous sintered compact, and manufacture of ferrous sintered compact |
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|---|---|
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ID=17144119
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|---|---|---|---|
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