JP6782749B2 - オーステナイト系ステンレス鋼の焼結方法 - Google Patents
オーステナイト系ステンレス鋼の焼結方法 Download PDFInfo
- Publication number
- JP6782749B2 JP6782749B2 JP2018207935A JP2018207935A JP6782749B2 JP 6782749 B2 JP6782749 B2 JP 6782749B2 JP 2018207935 A JP2018207935 A JP 2018207935A JP 2018207935 A JP2018207935 A JP 2018207935A JP 6782749 B2 JP6782749 B2 JP 6782749B2
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- JP
- Japan
- Prior art keywords
- stainless steel
- sintering
- austenitic stainless
- ferrite
- nitrogen
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000005245 sintering Methods 0.000 title claims description 44
- 238000000034 method Methods 0.000 title claims description 42
- 229910000963 austenitic stainless steel Inorganic materials 0.000 title claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 89
- 229910052757 nitrogen Inorganic materials 0.000 claims description 47
- 229910000859 α-Fe Inorganic materials 0.000 claims description 45
- 229910045601 alloy Inorganic materials 0.000 claims description 35
- 239000000956 alloy Substances 0.000 claims description 35
- 229910001566 austenite Inorganic materials 0.000 claims description 31
- 229910052799 carbon Inorganic materials 0.000 claims description 25
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 24
- 239000000843 powder Substances 0.000 claims description 19
- 239000010410 layer Substances 0.000 claims description 16
- 239000012159 carrier gas Substances 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 9
- 239000002344 surface layer Substances 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 238000004320 controlled atmosphere Methods 0.000 claims description 3
- 238000001746 injection moulding Methods 0.000 claims description 3
- 238000000149 argon plasma sintering Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 238000001125 extrusion Methods 0.000 claims description 2
- 239000012071 phase Substances 0.000 description 13
- 239000000203 mixture Substances 0.000 description 12
- 238000009792 diffusion process Methods 0.000 description 9
- 239000007791 liquid phase Substances 0.000 description 9
- 229910001220 stainless steel Inorganic materials 0.000 description 9
- 238000005498 polishing Methods 0.000 description 7
- 230000008859 change Effects 0.000 description 6
- 238000010587 phase diagram Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000007790 solid phase Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000005261 decarburization Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000005291 magnetic effect Effects 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 238000005121 nitriding Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000011800 void material Substances 0.000 description 3
- 238000005275 alloying Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000001419 dependent effect Effects 0.000 description 2
- 230000001627 detrimental effect Effects 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 241000951471 Citrus junos Species 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000000172 allergic effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000010191 image analysis Methods 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000000386 microscopy Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 230000000930 thermomechanical effect Effects 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24942—Structurally defined web or sheet [e.g., overall dimension, etc.] including components having same physical characteristic in differing degree
- Y10T428/24983—Hardness
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Description
‐焼結温度で液相を形成する1種以上の元素を添加することによる焼結:従って液相は固体状態よりはるかに速い拡散経路を提供し、それにより焼締めが改善される。オーステナイト系ステンレス鋼では、例えば少量のホウ素を添加できる。しかし、液相焼結後、合金の微小構造及び組成は均質ではなく、耐腐食性だけでなく研磨にも問題がある。
‐超固相線液相焼結(SLPS):これは合金の固相線と液相線との間の温度で焼結して合金の液相部分を得る工程を含む。しかし、ステンレス鋼では、固相線と液相線との間の温度範囲が狭すぎてプロセスを制御できないため、この技術にはほとんど関心が向けられていない。更に、このタイプの焼結は粒子成長を高め、やはり研磨操作に有害である。
1)窒素キャリアガス(例えばN2)を含む雰囲気中で100%オーステナイト域の粉末を焼結する第1工程。粉末の直径は通常、D90であり、5〜100μmの間にある。この工程中、開口空隙が除去されるまで加工物を焼き締めている間、合金中の窒素濃度は固定する。所与の合金では、窒素濃度は窒素キャリアガスの温度及び分圧(≧0.1bar)に依存する。合金中の炭素濃度は、粉末中の初期炭素濃度、粉末形成プロセスに使用する有機結合剤からの残留物、及び焼結中の炭素と雰囲気との反応(酸素による炭素低減、脱炭等)に依存する。従って、炭素濃度(例えばCO、CH4)の調整、又は全圧(例えばAr)の調整のために、酸化物還元用の窒素キャリアガス(例えばH2)に加えて他のガスを使用することが可能である。通常、オーステナイト域におけるこの単一の焼結工程は、オーステナイト系ステンレス鋼を焼結するための従来技術において利用している。
A.合金がフェライト+オーステナイトの2相、又は完全フェライト構造を有するように温度を設定する。表面では、オーステナイト相を安定化させる窒素と炭素は固体への拡散により大気中に放出可能であり、また炭素と窒素の溶解度がフェライト中ではかなり低くなることからフェライト形成が容易になる。表面での拡散によっても窒素及び炭素濃度が減少しない芯部では、第1工程において空隙が閉鎖するので、合金組成は変化しないままである。好ましくは、フェライト+オーステナイトの2相又は完全フェライト構造が表面にあるように、そして完全オーステナイト構造が芯部にあるように温度を設定するが、最初の2焼結工程で使用した合金及びパラメータに応じて、この工程では少量のフェライトも芯部に形成することが可能である。
B.窒素キャリアガスの分圧を設定するか、又は窒素を含まない雰囲気中で作業して、脱窒により加工物の表面における窒素量を減少させ、それによりオーステナイト+フェライト又は完全フェライト表面構造を形成する。表面での拡散によっても窒素濃度が減少しない芯部では、合金組成は変化しないままで、構造は完全オーステナイトのままである。
C.もし合金がすでに炭素を含んでいれば、炭素キャリアガス、例えばCO又はCH4の分圧を、脱炭により、又はより簡単に脱炭雰囲気、例えばH2を用いることにより加工物の表面における炭素量を減少させるように設定する。その後、当該雰囲気は、合金が平衡状態でオーステナイト+フェライトの2相又は完全フェライト構造を有するように再度選択しなければならない。表面での拡散によっても炭素濃度が減少しない芯部では、合金組成は変化しないままで、構造は完全オーステナイトのままである。
D.溶液A、B及びCの任意の組み合わせを使用する。
要するに、この工程では、加工物の表面にフェライトを形成して非常に高密度な層を得ることが目的である。フェライトは、固体中の拡散現象である脱窒及び/又は脱炭により形成されることから、所与の組成ではフェライトを含むこの高密度層の厚さは、温度、工程時間ならびに窒素及び/又は炭素キャリアガスの分圧に依存する。表面での拡散によっても窒素及び炭素濃度が減少しない芯部では、第1工程において空隙が閉鎖したので、組成、ひいては構造は変化しないままである。しかし、第1工程と第2工程とで温度が異なると、組成は変化しないものの少量のフェライトが芯部中にも形成される可能性がある。
1)100%オーステナイト域で開口空隙が除去されるまで粉末を窒化し、焼き締める。窒素濃度を調整可能にするのは温度及び窒素分圧である。満足のいく粉末窒化に要する時間は粉末粒径に依存する。しかし、100ミクロン未満のD90の粒子の場合、また1000℃を超える温度の場合、窒化速度は比較的速く、すなわち1時間未満である。しかし、空隙が閉鎖するまで焼き締めることは長時間になり、通常、数時間を要する。このように、厚さ約10mmの試料を1150℃で3時間保持し、開口空隙が除去されるまで試料を焼き締めることにより、平衡状態で合金中の窒素含有量を0.75重量%に到達させた(図1A及び1Bの丸1)。
2)熱力学的平衡状態で、フェライト+オーステナイト2相構造を得るために温度を1220℃に上昇させる。この工程はこの温度で1時間要する。表面では、窒素が大気中に放出され、フェライト形成は迅速である(図1Aの丸2)。窒素濃度が低下していない芯部では、温度上昇にもかかわらず構造はオーステナイトのままである(図1Bの丸2)。
3)1100℃の低温、2時間の保持時間で再窒化することにより、表面に存在するフェライトを除去する(図1A及び1Bの丸3)。温度及び保持時間は表面のフェライトが完全に除去されるように設定する。
2 層
3 芯部
4 空隙
Claims (18)
- 芯部(3)と表面とに密度差があるニッケル非含有オーステナイト系ステンレス鋼製加工物(1)を製造する方法であって、制御された雰囲気中で行われる以下の工程:
1)オーステナイト構造を有する焼結合金を提供するか、又は粉末を提供し、前記粉末を焼結し、前記焼結合金を形成する工程であって、前記焼結合金の窒素含有量は、0.1重量%以上である;
2)前記焼結合金を処理して前記オーステナイト構造を、前記合金の表面層(2)上でフェライト構造又はフェライト+オーステナイト2相構造に転換する工程;
3)前記焼結合金を処理して、前記工程2)で得た前記フェライト又はフェライト+オーステナイト2相構造を前記オーステナイト構造に転換し、冷却後、前記工程2)及び3)で転換を行った前記層(2)が前記加工物(1)の前記芯部(3)の密度より高い密度を有する前記加工物(1)を形成する工程;
を含み、
前記オーステナイト系ステンレス鋼のニッケル含有量は0.5重量%以下であり、
前記加工物は時計又は宝飾品の部品用の加工物である
ことを特徴とする方法。 - 請求項1に記載の方法であって、
前記焼結合金の炭素含有量は0.1重量%以上である
ことを特徴とする方法。 - 請求項1又は2に記載の方法であって、前記工程2)及び3)は、温度を調整すること、前記雰囲気の窒素キャリアガスの分圧を調整すること、及び前記雰囲気の炭素キャリアガスの分圧を調製することの1つ以上を含む
ことを特徴とする方法。 - 前記工程2)及び3)を合わせた保持時間が20時間未満であることを特徴とする請求項1又は2又は3に記載の方法。
- 0.1重量%以上の前記窒素含有量は、前記焼結工程1)で、前記雰囲気の前記窒素キャリアガスの温度及び分圧を制御することにより設定することを特徴とする請求項3〜4のいずれか1項に記載の方法。
- 前記粉末焼結工程1)及び前記工程2)及び3)は同じサイクル中に連続的に行うことを特徴とする請求項1〜5のいずれか1項に記載の方法。
- 前記工程2)及び3)は別々のサイクルで行うことを特徴とする請求項1〜5のいずれか1項に記載の方法。
- 前記工程1の前記焼結合金は射出成形、押し出し成形、プレス成形又は他の製造法により事前に成形することを特徴とする請求項1〜7のいずれか1項に記載の方法。
- 前記工程1の前記焼結合金は放電プラズマ焼結(SPS)又はレーザー焼結により得られることを特徴とする請求項1〜8のいずれか1項に記載の方法。
- 窒素含有量が0.1重量%以上のニッケル非含有オーステナイト系ステンレス鋼製加工物(1)であって、前記加工物(1)には、前記加工物(1)の芯部(3)の密度より高い密度を有する表面層(2)が含まれ、
前記オーステナイト系ステンレス鋼のニッケル含有量は0.5重量%以下であり、
前記加工物は時計又は宝飾品の部品用の加工物である
ことを特徴とする加工物(1)。 - 前記層(2)の厚さは20μm以上であることを特徴とする請求項10に記載の加工物(1)。
- 前記層(2)の厚さは50μm以上であることを特徴とする請求項10に記載の加工物(1)。
- 前記層(2)の厚さは0.75mm未満であることを特徴とする請求項10又は11又は12に記載の加工物(1)。
- 前記層(2)の厚さは0.5mm未満であることを特徴とする請求項10又は11又は12に記載の加工物(1)。
- 前記層(2)の密度は99〜100%であることを特徴とする請求項10〜14のいずれか1項に記載の加工物(1)。
- 前記オーステナイト系ステンレス鋼の炭素と窒素との合計含有量は0.2重量%以上であることを特徴とする請求項10〜15のいずれか1項に記載の加工物(1)。
- 前記オーステナイト系ステンレス鋼の平均粒径は300μm未満であることを特徴とする請求項10〜16のいずれか1項に記載の加工物(1)。
- 前記オーステナイト系ステンレス鋼の平均粒径は50μm未満であることを特徴とする請求項10〜16のいずれか1項に記載の加工物(1)。
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