JP5339770B2 - Method for manufacturing sintered body - Google Patents
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- JP5339770B2 JP5339770B2 JP2008115134A JP2008115134A JP5339770B2 JP 5339770 B2 JP5339770 B2 JP 5339770B2 JP 2008115134 A JP2008115134 A JP 2008115134A JP 2008115134 A JP2008115134 A JP 2008115134A JP 5339770 B2 JP5339770 B2 JP 5339770B2
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- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 238000000034 method Methods 0.000 title description 2
- 239000002245 particle Substances 0.000 claims description 67
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 39
- 239000000843 powder Substances 0.000 claims description 28
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 24
- 239000002994 raw material Substances 0.000 claims description 22
- 238000005245 sintering Methods 0.000 claims description 20
- 239000010949 copper Substances 0.000 claims description 13
- 238000000465 moulding Methods 0.000 claims description 12
- 239000011812 mixed powder Substances 0.000 claims description 7
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 238000004663 powder metallurgy Methods 0.000 claims description 3
- 239000000956 alloy Substances 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 5
- 229910017309 Mo—Mn Inorganic materials 0.000 description 4
- 238000005275 alloying Methods 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 229910020630 Co Ni Inorganic materials 0.000 description 1
- 229910002440 Co–Ni Inorganic materials 0.000 description 1
- 229910003296 Ni-Mo Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
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Description
本発明は、焼結原料粉末を用いた焼結体の製造方法に関する。
The present invention relates to a method for producing a sintered body using sintered raw material powder.
焼結体の強度と靭性を向上させるためにＮｉを添加した材料が、特許文献１〜５として従来から知られている。
特許文献１には、Ｆｅ−Ｃ−Ｃｕ−Ｎｉ−Ｍｏ系の焼結原料粉末が記載され、特にＦｅ粒子の表面に合金元素粒子を拡散せしめる際にＦｅ粒子が硬化して圧縮性が低下するのを防止するため、Ｆｅ粒子表面に合金元素粒子を拡散合金化させずに、潤滑剤とバインダの共溶融物を用いて合金元素粒子を付着させることが記載され、更に、合金元素粒子の粒径は４５μｍ以下、好ましくは１５μｍ以下のものを６０％以上とすることが記載されている。
Conventionally, materials added with Ni to improve the strength and toughness of the sintered body are known as Patent Documents 1 to 5.
Patent Document 1 describes an Fe—C—Cu—Ni—Mo-based sintering raw material powder, and particularly when the alloy element particles are diffused on the surface of the Fe particles, the Fe particles are cured and the compressibility is lowered. In order to prevent this, it is described that the alloy element particles are adhered to the Fe particle surface by using a co-melt of a lubricant and a binder without diffusion alloying the alloy element particles. It is described that the diameter is 45 μm or less, preferably 15 μm or less, and 60% or more.
特許文献２には、Ｆｅ−Ｍｏ−Ｍｎ系の焼結原料粉末にＮｉ粉末を添加する内容が記載され、特に、予合金化法における圧縮性の低下を防止するため、添加するＮｉの平均粒径をＦｅ−Ｍｏ−Ｍｎ系予合金粉末の平均粒径の１／１０以下にすることが提案されている。 Patent Document 2 describes the content of adding Ni powder to a Fe—Mo—Mn-based sintered raw material powder, and in particular, to prevent a decrease in compressibility in the prealloying method, the average grain of Ni to be added It has been proposed that the diameter be 1/10 or less of the average particle diameter of the Fe—Mo—Mn-based prealloy powder.
特許文献３には、Ｆｅ−Ｍｏ−Ｍｎ系の焼結原料粉末にＮｉ粉末を添加する内容が記載され、特にＮｉの合金化による圧縮性の低下を防止するため、Ｆｅ粉末を平均粒径が５０〜８０μｍの粗粉末と平均粒径が２０μｍ以下の微粉末の組み合わせとし、圧粉成形体を成形する際の圧縮性を改善することが提案されている。 Patent Document 3 describes the content of adding Ni powder to an Fe—Mo—Mn-based sintered raw material powder, and in particular, to prevent a decrease in compressibility due to Ni alloying, the Fe powder has an average particle size. It has been proposed to use a combination of a coarse powder of 50 to 80 μm and a fine powder having an average particle size of 20 μm or less to improve the compressibility when molding a green compact.
特許文献４には、極めて熱膨張率が小さなＦｅ−Ｃｏ−Ｎｉ系のスーパーアンバー合金が記載され、原料粉末の平均粒径として５〜５０μｍのものが提案されている。 Patent Document 4 describes a Fe-Co-Ni superamber alloy having an extremely small thermal expansion coefficient, and a material powder having an average particle diameter of 5 to 50 μm is proposed.
特許文献５には、熱処理を施さなくて済む焼結原料粉末として、Ｆｅ−Ｎｉ−Ｃｒ−Ｍｏ−Ｍｎ系のものが開示され、ＮｉについてはＦｅ粉体を硬くして圧縮性を低下せしめるので、０．３〜２．５重量％添加することが開示されている。 Patent Document 5 discloses a Fe-Ni-Cr-Mo-Mn-based powder as a sintering raw material powder that does not need to be heat-treated. For Ni, the Fe powder is hardened and the compressibility is lowered. , 0.3 to 2.5% by weight is disclosed.
上述した何れの先行技術にあっても、焼結の際にＮｉをＦｅに拡散して合金化するのに長時間（通常３０分以上）必要になる。また、焼結後の機械的強度が十分とは言えず、更なる強度の向上が望まれる。 In any of the above-described prior arts, it takes a long time (usually 30 minutes or more) to diffuse Ni into Fe to form an alloy during sintering. Moreover, it cannot be said that the mechanical strength after sintering is sufficient, and further improvement in strength is desired.
上記課題を解決するため本発明に係る焼結体の製造方法は、Ｃ（黒鉛）：０．６００〜０．８２５mass％、Ｃｕ（銅）：０．９７５〜１．０２５mass％、Ｎｉ（ニッケル）：２．９０〜３．１０mass％、Ｆｅ（鉄）：残部である原料粉末を用い、日本粉末冶金工業規格（ＪＰＭＡ）ＳＭＦ５０４０相当で、引張強度が１３．８ＫＮ／ｍｍ ２ 以上の焼結体の製造方法であって、原料粉末としてＦｅ粒子の平均粒径は７５μｍ以上１００μｍ以下、Ｃｕ粒子は前記Ｆｅ粒子よりも小径で平均粒径は２５μｍ以上４５μｍ以下、Ｎｉ粒子の平均粒径は０．８以上１．５μｍ未満の原料粉末を準備する工程と、前記原料粉末を混合し原料混合粉末とする工程と、前記原料混合粉末を成形荷重３９２〜５８８Ｎ／ｍｍ ２ 、金型及び前記原料混合粉末の温度８０〜１００℃として所定の形状に成形する工程と、焼結温度を１０７０〜１２５０℃、焼結時間を２０分以下として焼結を行う工程と、からなることを特徴とする。
In order to solve the above-mentioned problems, the manufacturing method of the sintered body according to the present invention is as follows: C ( graphite ): 0.600 to 0.825 mass%, Cu (copper): 0.975 to 1.025 mass%, Ni (nickel) : 2.90-3.10 mass%, Fe (iron): Using the remaining raw material powder, equivalent to Japan Powder Metallurgy Industry Standard (JPMA) SMF5040, with a tensile strength of 13.8 KN / mm 2 or more. In the manufacturing method, the average particle size of Fe particles as raw material powder is 75 μm or more and 100 μm or less, the Cu particles are smaller than the Fe particles, the average particle size is 25 μm or more and 45 μm or less, and the average particle size of Ni particles is 0.8. A step of preparing a raw material powder of less than 1.5 μm, a step of mixing the raw material powder to form a raw material mixed powder, a molding load of 392 to 588 N / mm 2 , a mold and the raw material mixed powder Temperature 8 A step of forming a predetermined shape as to 100 ° C., the sintering temperature 1070-1250 ° C., and wherein the step of performing sintering sintering time as 20 minutes or less, in that it consists of.
本願発明の焼結原料粉末の基本的な成分割合は、日本粉末冶金工業会規格（ＪＰＭＡ）のＳＭＦ５０４０に相当する。
Ｃ（炭素）は、焼結体の強度を高めるために添加するものであり、０．６００mass％未満では強度が不足し、０．８２５mass％を超えると過剰なＣが析出するので、上記の範囲とする。
Ｃｕ（銅）は、焼結体の強度を高めるために添加するものであり、０．９７５mass％未満では強度が不足し、１．０２５mass％を超えてもそれ以上の効果が期待できないので、上記の範囲とする。
Ｎｉ（ニッケル）は、焼結体の強度と靭性を高めるために添加するものであり、２．９０mass％未満では強度と靭性が不足し、３．１０mass％を超えてもそれ以上の効果が期待できないので、上記の範囲とする。
The basic component ratio of the sintered raw material powder of the present invention corresponds to SMF5040 of the Japan Powder Metallurgy Association (JPMA) standard.
C (carbon) is added to increase the strength of the sintered body. If the amount is less than 0.600 mass%, the strength is insufficient, and if it exceeds 0.825 mass%, excess C is precipitated. And
Cu (copper) is added to increase the strength of the sintered body. The strength is insufficient if it is less than 0.975 mass%, and no further effect can be expected even if it exceeds 1.025 mass%. The range.
Ni (nickel) is added to increase the strength and toughness of the sintered body. If it is less than 2.90 mass%, the strength and toughness are insufficient, and even if it exceeds 3.10 mass%, further effects are expected. Since this is not possible, the above range is used.
そして、本願発明の特徴となる点は、Ｆｅ粒子の平均粒径を１００μｍ以下、Ｃｕ粒子の平均粒径をＦｅ粒子よりも小径で４５μｍ以下、Ｎｉ粒子の平均粒径を０．８〜１．５μｍとした点にある。
各粒子の粒径を上記の範囲とすることで、Ｆｅ粒子の間にＣｕ粒子が充填され、Ｃｕ粒子とＦｅ粒子の間にＮｉ粒子が充填され、空隙率の低い焼結体が得られる。
また、Ｎｉ粒子の平均粒径を０．８〜１．５μｍとすることで、焼結（Ｎｉの合金化）に要する時間を大幅に短縮することができる。
The features of the present invention are that the average particle size of Fe particles is 100 μm or less, the average particle size of Cu particles is 45 μm or less smaller than the Fe particles, and the average particle size of Ni particles is 0.8 to 1. The point is 5 μm.
By setting the particle size of each particle within the above range, Cu particles are filled between Fe particles, Ni particles are filled between Cu particles and Fe particles, and a sintered body having a low porosity is obtained.
Further, by setting the average particle size of Ni particles to 0.8 to 1.5 μm, the time required for sintering (Ni alloying) can be greatly shortened.
本発明に係る焼結体の製造方法は、上記の構成からなる焼結原料粉末を所定の形状に成形した後に焼結する。そして、前記成形は成形荷重３９２〜５８８Ｎ／ｍｍ２、成形温度８０〜１００℃とし、焼結温度は１０７０〜１２００℃、焼結時間は２０分以下とする。 In the method for producing a sintered body according to the present invention, the sintering raw material powder having the above structure is formed into a predetermined shape and then sintered. The molding is performed with a molding load of 392 to 588 N / mm 2 , a molding temperature of 80 to 100 ° C., a sintering temperature of 1070 to 1200 ° C., and a sintering time of 20 minutes or less.
成形時に金型並びに材料粉末を８０〜１００℃に加熱しておくことで、成形荷重が低減でき、プレス機によって成形できる素材のサイズを大きくすることができる。先行技術に開示された合金化粉末は、純鉄粉に比べて硬度が高くなっており、金型の磨耗を引き起こし、また変形しにくいので成形荷重をより高めなければならないが、本発明はこれを解消することができる。 By heating the mold and the material powder to 80 to 100 ° C. at the time of molding, the molding load can be reduced and the size of the material that can be molded by a press machine can be increased. Although the alloyed powder disclosed in the prior art has higher hardness than pure iron powder, it causes wear of the mold and is difficult to deform, so the molding load must be increased. Can be eliminated.
本発明に係る焼結原料粉末によれば、焼結前の圧粉成形体の充填密度を高くすることができるので、焼結体の強度が向上する。また、Ｎｉ粒子の平均粒径を０．８〜１．５μｍとしたので、従来のＮｉ粒子（５μｍ）よりも比表面積が大きくなり、Ｎｉの拡散による合金化に要する時間が短くなる。 According to the sintered raw material powder according to the present invention, since the packing density of the green compact before sintering can be increased, the strength of the sintered body is improved. Further, since the average particle diameter of Ni particles is set to 0.8 to 1.5 μm, the specific surface area becomes larger than that of conventional Ni particles (5 μm), and the time required for alloying by diffusion of Ni is shortened.
以下に本発明の実施例を説明する。図１はＮｉ粒子径と焼結体の強度との関係を示すグラフ、図２（ａ）〜（ｅ）はＮｉ粒子径と焼結拡散状態との関係を示す顕微鏡写真である。 Examples of the present invention will be described below. FIG. 1 is a graph showing the relationship between the Ni particle diameter and the strength of the sintered body, and FIGS. 2A to 2E are micrographs showing the relationship between the Ni particle diameter and the sintered diffusion state.
先ず、以下の成分割合の焼結原料粉末を用意する。
Ｆｅ：９５．３５mass％
Ｃｕ： １．０mass％
Ｃ ： ０．６５mass％
Ｎｉ： ３．０mass％
First, a sintering raw material powder having the following component ratios is prepared.
Fe: 95.35 mass%
Cu: 1.0 mass%
C: 0.65 mass%
Ni: 3.0 mass%
前記各成分を構成する粒子の平均粒径は以下の通りである。
Ｆｅ粒子：７５μｍ
Ｃｕ粒子：２５μｍ
Ｎｉ粒子：０．８μｍ、１μｍ、２μｍ、３μｍ、４μｍ、５μｍ
Ｎｉ粒子については、上記の６種類の粒径のものを用意し、各粒径ごとに成形及び焼結を行った。
尚、Ｃについては焼結の際にＦｅに侵入する侵入型元素であるので、一般的な粒径（５μｍ）の黒鉛を用いた。
The average particle size of the particles constituting each component is as follows.
Fe particles: 75 μm
Cu particles: 25 μm
Ni particles: 0.8 μm, 1 μm, 2 μm, 3 μm, 4 μm, 5 μm
About Ni particle | grains, the thing of said 6 types of particle size was prepared, and it shape | molded and sintered for every particle size.
Since C is an interstitial element that enters Fe during sintering, graphite having a general particle size (5 μm) was used.
上記の混合粉体１００に対し潤滑剤を０．７５mass％添加し、偏りがないように混合し、この混合粉体を成形金型に充填し、成形圧力４９０Ｎ／ｍｍ２、成形温度９０℃で、成形体を形成した。成形体はＮｉ粒子の粒径ごとに６種類作成した。 0.75 mass% of lubricant is added to the above mixed powder 100 and mixed so as not to be biased, and this mixed powder is filled in a molding die, at a molding pressure of 490 N / mm 2 and a molding temperature of 90 ° C. A molded body was formed. Six types of compacts were prepared for each Ni particle size.
次いで、上記成形体を焼結温度を１１５０℃、焼結時間を２０分として焼結を行った。焼結体の強度とＮｉ粒子の粒径との関係を図１に示す。また、Ｎｉ粒子の各粒径ごとの組織の顕微鏡写真を図２（ａ）〜（ｅ）に示す。 Subsequently, the compact was sintered at a sintering temperature of 1150 ° C. and a sintering time of 20 minutes. The relationship between the strength of the sintered body and the particle size of the Ni particles is shown in FIG. Moreover, the micrograph of the structure | tissue for every particle size of Ni particle | grains is shown to Fig.2 (a)-(e).
図１から、焼結体の強度とＮｉ粒子の粒径とは比例関係にあり、ギヤなどを焼結体で構成した場合に要求される強度として、１３．８ＫＮを目標値とすると、Ｎｉ粒子の粒径は０．８〜１．５μｍとすべきことが分かる。 From FIG. 1, the strength of the sintered body and the particle size of the Ni particles are in a proportional relationship, and when the target strength is 13.8 KN when the gear or the like is made of a sintered body, the Ni particles It can be seen that the particle size should be 0.8-1.5 μm.
また、図２からＮｉ粒子の粒径が１μｍ、２μｍの場合には、Ｎｉの偏析は見られず、これが強度向上に寄与していることが、推察できる。 Further, it can be inferred from FIG. 2 that when the particle size of the Ni particles is 1 μm and 2 μm, no segregation of Ni is observed and this contributes to the strength improvement.
Claims (1)
原料粉末としてＦｅ粒子の平均粒径は７５μｍ以上１００μｍ以下、Ｃｕ粒子は前記Ｆｅ粒子よりも小径で平均粒径は２５μｍ以上４５μｍ以下、Ｎｉ粒子の平均粒径は０．８以上１．５μｍ未満の原料粉末を準備する工程と、
前記原料粉末を混合し原料混合粉末とする工程と、
前記原料混合粉末を成形荷重３９２〜５８８Ｎ／ｍｍ２、金型及び前記原料混合粉末の温度８０〜１００℃として所定の形状に成形する工程と、
焼結温度を１０７０〜１２５０℃、焼結時間を２０分以下として焼結を行う工程と、
からなることを特徴とする焼結体の製造方法。 C ( graphite ): 0.600 to 0.825 mass%, Cu (copper): 0.975 to 1.025 mass%, Ni (nickel): 2.90 to 3.10 mass%, Fe (iron): the balance A method for producing a sintered body having a tensile strength of 13.8 KN / mm 2 or more, equivalent to Japan Powder Metallurgy Industry Standard (JPMA) SMF5040 , using raw material powder ,
The average particle size of Fe particles as raw material powder is 75 μm or more and 100 μm or less, the Cu particles are smaller than the Fe particles, the average particle size is 25 μm or more and 45 μm or less, and the average particle size of Ni particles is 0.8 or more and less than 1.5 μm Preparing a raw material powder;
Mixing the raw material powder to obtain a raw material mixed powder;
Forming the raw material mixed powder into a predetermined shape with a molding load of 392 to 588 N / mm 2 , a mold and a temperature of the raw material mixed powder of 80 to 100 ° C .;
A step of sintering at a sintering temperature of 1070 to 1250 ° C. and a sintering time of 20 minutes or less;
The manufacturing method of the sintered compact characterized by comprising.
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| US5154881A (en) * | 1992-02-14 | 1992-10-13 | Hoeganaes Corporation | Method of making a sintered metal component |
| JPH07173503A (en) * | 1993-11-04 | 1995-07-11 | Kobe Steel Ltd | Binder for powder metallurgy and powdery mixture for powder metallurgy |
| JPH07228901A (en) * | 1994-02-16 | 1995-08-29 | Kobe Steel Ltd | Method for adjusting apparent density of mixed powder for powder metallury and mixed powder for powder metallurgy |
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| JP2002173703A (en) * | 2000-12-01 | 2002-06-21 | Univ Nihon | Method for manufacturing sintered compact of metal powder |
| JP2005154828A (en) * | 2003-11-25 | 2005-06-16 | Mitsubishi Materials Corp | Raw material powder for warm compacting, and warm compacting method |
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