JPWO2005087418A1 - 焼結工具とその製造方法 - Google Patents
焼結工具とその製造方法 Download PDFInfo
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- JPWO2005087418A1 JPWO2005087418A1 JP2006511012A JP2006511012A JPWO2005087418A1 JP WO2005087418 A1 JPWO2005087418 A1 JP WO2005087418A1 JP 2006511012 A JP2006511012 A JP 2006511012A JP 2006511012 A JP2006511012 A JP 2006511012A JP WO2005087418 A1 JPWO2005087418 A1 JP WO2005087418A1
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- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/02—Pretreatment of the material to be coated
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C12/00—Solid state diffusion of at least one non-metal element other than silicon and at least one metal element or silicon into metallic material surfaces
- C23C12/02—Diffusion in one step
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
- C23C26/02—Coating not provided for in groups C23C2/00 - C23C24/00 applying molten material to the substrate
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- C—CHEMISTRY; METALLURGY
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- C23C30/00—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process
- C23C30/005—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process on hard metal substrates
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/02—Pretreatment of the material to be coated
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/241—Chemical after-treatment on the surface
- B22F2003/242—Coating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
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Abstract
Description
以下、本発明を具体例に基づき、詳細に説明する。
この時の被膜厚さの調整は、ガス濃度、キャリアガス流量、加熱温度、加熱時間、等によって制御される。
これらのことから、WC-Co 系合金におけるケイ素拡散熱処理温度は、1250〜1320℃ が利用され、WC-Ni 系合金では1150〜1350℃ の範囲が利用される。
上記の実施例試料と比較例試料は、次の条件で拡散熱処理を行った。試料は、真空炉中で保持して、炉内圧40〜80Paに制御し、昇温速度5℃/minで加熱し、1200℃、1250℃及び1280℃の3水準の熱処理温度に3時間保持し、拡散熱処理を行い、後に炉令した。
図6に示すCVD装置を用いた。3塩化ホウ素[BCl3]と、メタン[CH4]、水素[H2]のガスボンベ11,12,13から流量計3および調整弁4を介して加熱炉1に調製されたガスが供給される。なお、加熱炉1には水封ポンプ2が連結されており、加熱炉内を所望の減圧に設定できるようになっている。この加熱炉1内に、実施例1で用いた2種類の焼結体をセットしておき、下表に示す化学蒸着条件でCVD処理を行った。処理後の焼結体表面のB4C成膜厚さを確認したところ、およそ12〜15μmであった。
この実施例では、減圧CVD処理であったが、さらに膜厚を増大させるには、熱CVD法やレーザーCVD法を用いればよく、所望の被覆層厚さが得られる。
表B 4 C蒸着条件
上記被膜層は上記実施例1〜3と同様の熱処理により、所定の拡散熱処理効果が認められた。
市販の平均粒度 5.7 μm の WC 粉と 1.3 μm の Co 粉、1.5 μm の Ni 粉、さらに Cr-C 粉を用いて、WC-13%Co-2%Ni-1%Cr [ 15LB ]と、WC-18%Co-4%Ni-1.5%Cr [ 22HB ]組成に調合、混合した。得られた混合粉末から、実施例1と同形状の圧粉成型体を作製した後、真空中で 1380℃×1 Hr の液相焼結を行い、それぞれの焼結素材を得た。
次に、熱処理のケイ素源として、炭化ケイ素 SiC を用いて被覆材を調整した。調整の方法は実施例1と同様に行い、15% SiC 含有エタノール塗剤を準備した。浸漬法により焼結素材表面に被覆し、乾燥し、拡散熱処理を行った。熱処理温度は 1300℃×3 Hr とした。尚、被覆処理をしない素材そのままの試料も比較評価を行った。
熱処理後の試料は、長さ 15 mm の位置で切断し、切断面を研磨後、断面組織観察を行い、その後、表面から深さを変えてビッカース硬度計による硬さ測定を行った。
組織観察の結果については、表層部深さ 2 mm 程度までが WC 粒子の分布密度に向上が認められ、それより内部では明らかにバインダ金属が多い組織形態であった。
硬度測定の結果は、表4および図7に示す。
表4
図7から明らかなように、粗粒 WC を使用しているため、硬さとしては比較的低い値であるが、内質部と比較すると、表層部硬さは顕著な増大が認められた。
又、ケイ素の拡散深さは、硬さ傾斜部と見なすと、ホウ素拡散素材よりも小さく、これはホウ素とケイ素の元素特性の違いによるものと考えられた。しかしながら、バインダ金属の拡散移動はホウ素と同様の挙動を示すことが確認され、温間・熱間工具に致命的なヒートクラックの抑制に対する表面圧縮残留応力の効果、並びに耐熱性、耐酸化性が付与されることは、高温領域に適用される工具として極めて有用な特徴を有するものである。
又、被覆材として、SiB6 を使用すれば、ホウ素とケイ素の両特性が複合した表層部特性が得られる。
Claims (13)
- 硬質の炭化物、窒化物若しくは炭窒化物を含む硬質粒子と、バインダ金属として鉄族金属と、から成る焼結工具において、
上記の焼結工具が、ホウ素Bおよび/またはケイ素Siを重量で0.010〜2.0%の範囲で含む表層部を有し、該表層部が、内質部よりも高い分布密度の硬質粒子を有することを特徴とする焼結工具。 - 表層部が、実質的に、硬質粒子相と、ホウ素および/またはケイ素Siとバインダ金属との化合物であるホウ化物および/またはケイ化物相と、から成り、焼結工具中該表層部より内側の内質部が、実質的に硬質粒子相とバインダ金属相とから成る請求項1に記載の焼結工具。
- 内質部中の鉄族金属と硬質粒子との含有量の重量比が、5:95ないし40:60の範囲にある請求項1又は2に記載の焼結工具。
- バインダ金属がCo若しくはNiを含み、
表層部のホウ化物および/またはケイ化物相がCo若しくはNiを含む請求項2又は3に記載の焼結工具。 - 表層部の表面から深さ0.5mmまでの範囲でのバインダ金属の含有量が、重量で2%以下である請求項1ないし4いずれかに記載の焼結工具。
- 表層部が、内質部より、互いに隣接する硬質粒子の間の平均間隔が小さいことを特徴とする請求項1ないし5いずれかに記載の焼結工具。
- 表層部の硬質粒子の粒子径分布が、内質部と実質的に同じである請求項1ないし6いずれかに記載の焼結工具。
- 硬質粒子と鉄族のバインダ金属とから焼結して成る焼結工具の製造方法において、製造方法が、
硬質粒子と鉄族のバインダ金属との混合粉末を圧縮成形して所望形状の圧粉体とし、次いで、該圧粉体を焼結により焼結体とすること、
該焼結体の表面にホウ素および/またはケイ素被覆層を形成すること、及び
該ホウ素および/またはケイ素被覆層を有する上記焼結体を、真空中または不活性ガス雰囲気中で、上記焼結体の液相温度より低く、且つ、該焼結体でホウ素および/またはケイ素を含有する融液を形成するに必要な温度の範囲で、加熱保持する熱処理をすること、
を含み、
上記の熱処理過程で、ホウ素および/またはケイ素被覆層中のホウ素および/またはケイ素を焼結体の表層部に拡散させて、表層部中のホウ素および/またはケイ素含有融液を内質部に拡散移動させ、焼結体の表層部の硬質粒子の分布密度を内質部よりも高くしたことを特徴とする焼結工具の製造方法。 - 表層部に、ホウ素Bおよび/またはケイ素を重量で0.050〜1.0%の範囲で含有させる請求項8に記載の製造方法。
- 表層部は、硬質粒子の粒径分布が、内質部と実質的に同じである請求項8又は9に記載の製造方法。
- 上記のホウ素および/またはケイ素被覆材が、ホウ素および/またはケイ素の酸化物、窒化物及び炭化物のいずれか1種を含む請求項8ないし10いずれかに記載の製造方法。
- 被覆層中ホウ素および/またはケイ素が、金属ホウ素および/またはケイ素元素に換算して、被覆面に対して5.0〜60mg/cm2の範囲にあることを特徴とする請求項8ないし11いずれかに記載の製造方法。
- 被膜層形成工程がa)焼結体表面にホウ素および/またはケイ素を含む塗剤を被覆するか、b)焼結体をホウ素又はケイ素の塩化物、フッ化物、水素化物、又は有機金属化合物のガス気流中で加熱して焼結体表面にホウ素又はケイ素を蒸着被覆するか、あるいはc)焼結体に半溶融状態にまで加熱したホウ素又はケイ素の化合物を溶射して焼結体表面にホウ素又はケイ素を被覆する工程からなる請求項8記載の焼結工具の製造方法。
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