JP4927517B2 - Method for regenerating hard film coated tool and method for regenerating hard film coated mold - Google Patents
Method for regenerating hard film coated tool and method for regenerating hard film coated mold Download PDFInfo
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- 238000000034 method Methods 0.000 title claims description 26
- 230000001172 regenerating effect Effects 0.000 title claims description 11
- 239000007888 film coating Substances 0.000 claims description 34
- 238000009501 film coating Methods 0.000 claims description 34
- 238000000576 coating method Methods 0.000 claims description 28
- 229910052736 halogen Inorganic materials 0.000 claims description 28
- 150000002367 halogens Chemical class 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 25
- 239000012298 atmosphere Substances 0.000 claims description 24
- 150000001875 compounds Chemical class 0.000 claims description 17
- 239000003085 diluting agent Substances 0.000 claims description 10
- 150000002366 halogen compounds Chemical class 0.000 claims 2
- 239000007789 gas Substances 0.000 description 75
- 239000000463 material Substances 0.000 description 29
- 239000011248 coating agent Substances 0.000 description 24
- 239000002585 base Substances 0.000 description 13
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 12
- 239000000126 substance Substances 0.000 description 10
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 8
- -1 CrSiN Chemical compound 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 238000005240 physical vapour deposition Methods 0.000 description 7
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 6
- 239000000460 chlorine Substances 0.000 description 6
- 238000005520 cutting process Methods 0.000 description 6
- 229910052731 fluorine Inorganic materials 0.000 description 6
- 239000011737 fluorine Substances 0.000 description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 5
- 229910010037 TiAlN Inorganic materials 0.000 description 5
- 229910001315 Tool steel Inorganic materials 0.000 description 5
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 5
- 229910052794 bromium Inorganic materials 0.000 description 5
- 229910052801 chlorine Inorganic materials 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000012299 nitrogen atmosphere Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 4
- 229910008482 TiSiN Inorganic materials 0.000 description 4
- 238000010828 elution Methods 0.000 description 4
- 150000004820 halides Chemical class 0.000 description 4
- 238000007733 ion plating Methods 0.000 description 4
- 230000008929 regeneration Effects 0.000 description 4
- 238000011069 regeneration method Methods 0.000 description 4
- 230000003746 surface roughness Effects 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 3
- 229910052740 iodine Inorganic materials 0.000 description 3
- 239000011630 iodine Substances 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- QRXWMOHMRWLFEY-UHFFFAOYSA-N isoniazide Chemical compound NNC(=O)C1=CC=NC=C1 QRXWMOHMRWLFEY-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 150000001247 metal acetylides Chemical class 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 229910000997 High-speed steel Inorganic materials 0.000 description 1
- 229910020968 MoSi2 Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 1
- 229910001854 alkali hydroxide Inorganic materials 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 238000010273 cold forging Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000002230 thermal chemical vapour deposition Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 238000001947 vapour-phase growth Methods 0.000 description 1
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- Chemical Vapour Deposition (AREA)
Description
本発明は、切削工具や成形工具等のＰＶＤやＣＶＤによる硬質皮膜コーティングが施された工具の再生方法および硬質皮膜コーティングされた金型の再生方法に関するものである。
The present invention relates to a method for regenerating a tool coated with a hard film by PVD or CVD, such as a cutting tool or a forming tool, and a method for regenerating a mold coated with a hard film .
近年、高速度工具鋼や超硬合金の表面に窒化チタンや炭化チタンなどＴｉ系皮膜など、またはＣｒＮ，ＡｌＮ，ＳｉＮ，ＢＮ，ＴｉＡｌＮ，ＴｉＣＮ，ＣｒＡｌＮ，ＴｉＳｉＮ，ＣｒＳｉＮなどの膜やＴｉＮ／ＴｉＣＮ／ＴｉＮ，ＴｉＮ／ＴｉＡｌＮなどの多層膜を硬質皮膜コーティングすることで、耐摩耗性を向上させた切削工具が多用されるようになっている。また、切削工具だけでなく、ダイス鋼の表面に同様の硬質皮膜コーティングを施し、ダイス、パンチ、金型等の成形工具も多く用いられるようになっている。 In recent years, Ti-based coatings such as titanium nitride and titanium carbide on the surface of high-speed tool steel and cemented carbide, or films such as CrN, AlN, SiN, BN, TiAlN, TiCN, CrAlN, TiSiN, CrSiN, and TiN / TiCN / Cutting tools with improved wear resistance have been widely used by coating hard films with multilayer films such as TiN and TiN / TiAlN. In addition to cutting tools, the same hard film coating is applied to the surface of die steel, and many forming tools such as dies, punches, and dies are used.
このような工具類は、使用するにしたがってコーティングが劣化したり摩滅したりするので、必要に応じてコーティングを除去して再研磨や再コーティングを行って再生し、新品と同様の状態にしてリサイクルして利用する方法が行われつつある。 Such tools will deteriorate or wear out as you use them, so if necessary, remove the coating, re-grind and re-coat it, recycle it, and recycle it in the same state as a new one. The method of using it is being carried out.
このようなリサイクル利用におけるＴｉ系皮膜などの除去は、例えば、下記の特許文献１に開示されているように、過酸化水素や水酸化アルカリを含む薬液に浸漬することにより除去することが行われている（例えば、下記の特許文献１）。また、このような薬液処理以外に、高濃度のフッ素系ガスを含むプラズマ中にコーティング工具類を晒すことにより窒化物コーティングを除去する方法も提案されている（例えば、下記の特許文献２）
しかしながら、薬液への浸漬で硬質皮膜コーティングを除去するには、少なくとも１２時間以上浸漬しておく必要があり、極めて時間効率が悪いという問題がある。しかも、母材が超硬合金からなる場合、薬液への浸漬によってＣｏ等の溶出が起こり、母材を傷め表面粗れを引き起こすため、超硬合金製の工具類には実質的に薬液処理を適用することができなかった。一方、プラズマ雰囲気内に工具類を晒す方法では、高価なプラズマ処理設備が必要になるため、結果的に処理コストが跳ね上がってしまうという問題がある。 However, in order to remove the hard coating by immersion in a chemical solution, it is necessary to soak for at least 12 hours or more, and there is a problem that time efficiency is extremely poor. In addition, when the base material is made of a cemented carbide, elution of Co or the like occurs due to immersion in the chemical solution, which damages the base material and causes surface roughness, so that the cemented carbide tools are substantially treated with the chemical solution. Could not be applied. On the other hand, the method of exposing tools to the plasma atmosphere requires expensive plasma processing equipment, resulting in a problem that the processing cost increases as a result.
本発明はこのような事情に鑑みなされたものであり、母材を傷めることなく安価かつ容易に硬質皮膜コーティングを除去して硬質皮膜コーティングされた工具や金型の再生を行うことができる硬質皮膜コーティングされた工具の再生方法および硬質皮膜コーティングされた金型の再生方法の提供を目的とする。
The present invention has been made in view of such circumstances, and can remove a hard film coating inexpensively and easily without damaging the base material and can regenerate a hard film coated tool or mold. It is an object of the present invention to provide a method for regenerating a coated tool and a method for regenerating a hard film coated mold .
すなわち、本発明の硬質皮膜コーティングされた工具の再生方法は、ＰＶＤやＣＶＤによる硬質皮膜コーティングが施された工具を、プラズマ発生設備のない雰囲気炉で加熱し、
上記加熱した雰囲気炉内に、主成分ガスに希釈ガスを加えたプラズマを含まないハロゲン系化合物ガスを導入して上記ハロゲン系化合物ガスが存在する大気圧近傍の雰囲気中において工具を加熱保持し、
上記工具をプラズマ中に晒さないで、プラズマを含まないハロゲン系化合物ガスにより表面の硬質皮膜コーティングをハロゲン化物とすることにより除去し、
その後、硬質皮膜コーティングの再コーティング処理を行うことを要旨とする。
また、本発明の硬質皮膜コーティングされた金型の再生方法は、ＰＶＤやＣＶＤによる硬質皮膜コーティングが施された金型を、プラズマ発生設備のない雰囲気炉で加熱し、
上記加熱した雰囲気炉内に、主成分ガスに希釈ガスを加えたプラズマを含まないハロゲン系化合物ガスを導入して上記ハロゲン系化合物ガスが存在する大気圧近傍の雰囲気中において金型を加熱保持し、
上記金型をプラズマ中に晒さないで、プラズマを含まないハロゲン系化合物ガスにより表面の硬質皮膜コーティングをハロゲン化物とすることにより除去し、
その後、硬質皮膜コーティングの再コーティング処理を行うことを要旨とする。
That is, the method of reproducing the hard coating coated tool of the present invention, the tool hard film coating by PVD or CVD is performed, and heated in an atmosphere furnace without plasma generation equipment,
Into the heated atmospheric furnace, a halogen-based compound gas not containing a plasma in which a diluent gas is added to the main component gas is introduced to heat and hold the tool in an atmosphere near the atmospheric pressure where the halogen-based compound gas exists,
Without exposing the above tool to the plasma, removing the hard film coating on the surface with a halogen-based compound gas that does not contain plasma to remove it,
Then, the gist is to perform a re-coating treatment of the hard film coating.
Moreover, a hard film coated mold reproducing method of the present invention, a mold hard film coating is applied by PVD or CVD, and heated in an atmosphere furnace without plasma generation equipment,
Into the heated atmosphere furnace, a halogen-based compound gas not containing plasma in which a diluent gas is added to the main component gas is introduced, and the mold is heated and maintained in an atmosphere near the atmospheric pressure where the halogen-based compound gas exists. ,
Without exposing the above mold to the plasma, removing the hard film coating on the surface with a halogen-based compound gas that does not contain plasma to remove it,
Then, the gist is to perform a re-coating treatment of the hard film coating.
すなわち、本発明は、ＰＶＤやＣＶＤによる硬質皮膜コーティングが施された工具または金型を、ハロゲン系化合物ガスが存在する大気圧近傍の雰囲気中において加熱保持する。そして、表面の硬質皮膜コーティングをハロゲン化物とすることにより除去する。このため、従来の薬液処理に比べて大幅に短い時間で硬質皮膜コーティングを除去し、工具または金型の再生を行うことができる。そして、硬質皮膜コーティングが除去された工具または金型は、必要に応じて再研磨を行い、再コーティングを行って再利用することができる。また、本発明の硬質皮膜コーティングされた工具または金型の再生方法は、従来のようにプラズマ雰囲気ではなく、加熱雰囲気を利用するため、高価な設備が不要で極めて安価に再生処理を行うことができる。さらに、母材が超硬合金であっても従来の薬液処理のようにＣｏ溶出による母材の損傷や粗れが生じないため、再生後の金属部品の耐磨耗性等に悪影響を及ぼさない。 また、本発明は、上記加熱保持の際の圧力が大気圧近傍であるため、大気圧の加熱炉内をハロゲン系化合物ガスでパージして加熱保持すればよいことから、容易かつ安価に再生処理を行うことができる。
なお、本発明において「大気圧近傍」とは、−２００ＰａＧ〜２００ＰａＧの範囲内の圧力をいう。
That is, the present onset Ming, the tool or mold a hard film coating is applied by PVD or CVD, heat held in an atmosphere of near atmospheric pressure existing halogen-based compound gas. Then, the hard film coating on the surface is removed by using a halide. For this reason, the hard film coating can be removed and the tool or the mold can be regenerated in a significantly shorter time than the conventional chemical treatment. The tool or die hard film coating has been removed, have rows regrinding optionally, can be reused by performing recoat. In addition, the method for regenerating a hard film coated tool or mold according to the present invention uses a heating atmosphere instead of a plasma atmosphere as in the prior art, so that expensive equipment is not required and the regeneration process can be performed at a very low cost. it can. Furthermore, even if the base material is a cemented carbide, the base material is not damaged or roughened due to Co elution unlike the conventional chemical treatment, so it does not adversely affect the wear resistance of the metal parts after recycling. . Further, according to the present invention, since the pressure at the time of the heating and holding is near atmospheric pressure, the inside of the heating furnace at atmospheric pressure may be purged with a halogen-based compound gas and heated and held. It can be performed.
In the present invention, “near atmospheric pressure” refers to a pressure within a range of −200 PaG to 200 PaG.
また、上記加熱保持は工具または金型をプラズマ中に晒さないで行うため、高価なプラズマ発生設備が不要で、極めて安価に再生処理を行うことができる。
Also, the heat retained for performing not expose the tool or mold in the plasma, expensive plasma generating facility is not required, it can be performed very inexpensively reproduction process.
本発明において、上記加熱保持の時間は３０分以上である場合には、硬質皮膜コーティングを十分に除去することができる。
In the present invention, when the heating and holding time is 30 minutes or more, the hard film coating can be sufficiently removed.
本発明において、上記ハロゲン系ガスがＮＦ３系ガスである場合には、反応性、取り扱い性等の面で優れており、実用的である。 In the present invention, when the halogen-based gas is an NF 3 -based gas, it is excellent in terms of reactivity, handleability, etc., and is practical.
つぎに、本発明を実施するための最良の形態を説明する。 Next, the best mode for carrying out the present invention will be described.
本発明は、ＰＶＤやＣＶＤによる硬質皮膜コーティングが施された工具または金型を、ハロゲン系化合物ガスが存在する大気圧近傍の雰囲気中において加熱保持し、表面の硬質皮膜コーティングをハロゲン化物とすることにより除去する工程を備えている。
This onset Ming, the tool or mold a hard film coating is applied by PVD or CVD, and heated and held in an atmosphere of near atmospheric pressure existing halogen-based compound gas, the hard film coating the surface with a halide The process of removing by this is provided.
本発明が対象とするのは、例えば、バイト、スローアウェイチップ、リーマ、ドリル、エンドミル等の切削工具や、熱間鍛造金型、冷間鍛造金型、射出成形金型、引き抜き用ダイス、押出し用ダイス、プレス用ダイス、プレス用パンチ等の成形工具等の工具類や、一部の機械部品等をあげることができるが、これらに限定するものではない。
The present invention is directed are, for example, byte, indexable inserts, reamers, drills, and cutting tool such as an end mill, hot forging dies, cold forging dies, injection mold, drawing die, extrusion Tools such as forming dies such as dies for pressing, dies for pressing, and punches for pressing, and some machine parts can be exemplified, but the present invention is not limited thereto.
本発明が対象とする硬質皮膜コーティングは、例えば、チタン、タングステン、等の窒化物、炭化物、炭窒化物、ほう化物、酸化物等をあげることができる。具体的には、ＴｉＣ，ＴｉＮ，Ｔｉ（ＣＮ），ＴｉＢ２，ＴｉＡｌＮ，ＴｉＣｒＮ，ＴｉＳｉＮ，ＴｉＢ２ ，ＣｒＳｉＮ，ＷＣ，Ｗ２Ｃ，ＳｉＣ，ＳｉＮ，Ｓｉ３Ｎ４，ＳｉＯ２，ＢＮ，Ｃ−ＢＮ，ＭｏＳｉ２等各種のコーティング物質を対象とすることができる。これらのなかでも、工具類等に耐摩耗性を付与するための耐磨耗コーティング物質として、ＴｉＣ，ＴｉＮ，ＴｉＢ２，ＷＣ，Ｗ２Ｃ，ＳｉＣ等各種のコーティング物質を好適に対象とすることができる。
Hard film coatings to which the present invention is directed, for example, may be mentioned titanium, data tungsten, nitrides etc., carbides, carbonitrides, borides, oxides, and the like. Specifically, TiC, TiN, Ti (CN ), TiB 2, TiAlN, TiCrN, TiSiN, T iB 2, C rSiN, WC, W 2 C, SiC, SiN, Si 3 N 4, SiO 2, BN, Various coating materials such as C-BN and MoSi2 can be targeted. Among them, for as antiwear coating material for imparting wear resistance to the tool, and the like, TiC, TiN, T iB 2 , WC, W 2 C, and preferably subject the coating material such as SiC various be able to.
これらの硬質皮膜コーティングとしては、例えば真空蒸着、イオンプレーティング、スパッタリング等の物理蒸着法（ＰＶＤ法）、熱ＣＶＤ、プラズマＣＶＤ等の気相成長法等、各種の気相コーティング法により形成されたものを対象とすることができる。 These hard film coatings are formed by various vapor phase coating methods such as physical vapor deposition methods (PVD method) such as vacuum deposition, ion plating and sputtering, and vapor phase growth methods such as thermal CVD and plasma CVD. You can target things.
上記硬質皮膜コーティングが施される母材としては、例えば、切削用工具鋼、耐摩不変形用工具鋼、耐衝撃用工具鋼、熱間加工用工具鋼、高速度鋼等の各種工具鋼や、超硬合金等をあげることができる。特に、母材が超硬合金からなる場合には、Ｃｏの溶出による表面粗れのために薬液処理ができないので効果的である。 Examples of the base material on which the hard film coating is applied include, for example, various tool steels such as tool steel for cutting, tool steel for wear resistance, tool steel for impact resistance, tool steel for hot working, and high speed steel, Examples thereof include cemented carbide. In particular, when the base material is made of a cemented carbide, it is effective because chemical treatment cannot be performed due to surface roughness due to Co elution.
本発明に用いるハロゲン系ガスとしては、例えば、塩素系ガス、フッ素系ガス、臭素系ガス，ヨウ素系ガス等をあげることができる。 Examples of the halogen-based gas used in the present invention include a chlorine-based gas, a fluorine-based gas, a bromine-based gas, and an iodine-based gas.
上記塩素系ガスとしては、例えば、ＢＣｌ３ ，ＣＣｌ４等の塩素化合物からなる主成分ガスをＮ２ガス等の希釈ガスで希釈して塩素系ガスとして使用することができる。
As the chlorine-based gas, for example, a main component gas composed of a chlorine compound such as BCl 3 and C Cl 4 can be diluted with a diluent gas such as N 2 gas and used as a chlorine-based gas .
上記フッ素系ガスとしては、例えば、ＮＦ３，ＢＦ３，ＣＦ４、ＳＦ６，ＣＨＦ３，Ｃ２Ｆ６等のフッ素化合物からなる主成分ガスをＮ２ガス等の希釈ガスで希釈してフッ素系ガスとして使用することができる。これらフッ素系ガスに用いられる主成分ガスのうち、反応性、取り扱い性等の面でＮＦ３が最も優れており、実用的である。
Examples of the fluorine-based gas include fluorine by diluting a main component gas composed of a fluorine compound such as NF 3 , BF 3 , CF 4 , SF 6 , CHF 3 , C 2 F 6 with a diluent gas such as N 2 gas. It can be used as a system gas . Of the principal components gas used these fluorine-based gas, reactive, and is best NF 3 in terms of such handling properties, it is practical.
上記臭素系ガスとしては、例えば、ＨＢｒ，ＢＢｒ３，ＣＯＢｒ２，Ｓ２Ｂｒ２等の臭素化合物からなる主成分ガスをＮ２ガス等の希釈ガスで希釈して臭素系ガスとして使用することができる。
As the bromine-based gas, for example, a main component gas composed of a bromine compound such as HBr , BBr 3 , COBr 2 , S 2 Br 2 is diluted with a diluent gas such as N 2 gas and used as a bromine-based gas. Can do .
上記ヨウ素系ガスとしては、ＩＦ５、ＩＦ６、ＩＦ７、ＩＣｌ、ＩＣｌ３、ＩＢｒ、ＩＢｒ３等のインターハロゲン化合物、ＣＩＦ３、ＣＩ２Ｆ２、ＣＩ３Ｆ、ＣＩ４等の炭化物、ＳｉＩ４等のケイ化物、ＣＨ３Ｉ、ＣＨ３ＯＩ等のアルキル化合物やアルコキシ化合物、ＣＦ３Ｉ、ＨＩ等、室温領域で気体あるいは気化しやすい化合物等からなる主成分ガスをＮ２ガス等の希釈ガスで希釈してヨウ素系ガスとして使用することができる。
Examples of the iodine-based gas include interhalogen compounds such as IF 5 , IF 6 , IF 7 , ICl, ICl 3 , IBr, and IBr 3 , carbides such as CIF 3 , CI 2 F 2 , CI 3 F, and CI 4 , SiI silicides 4 such as CH 3 I, alkyl compounds and alkoxy compounds such as CH 3 OI, CF 3 I, H I , etc., the main component gas consisting of gas or vaporized easily compounds at room temperature region, such as N 2 gas It can be diluted with a diluent gas and used as iodine-based gas .
上記塩素系ガス、フッ素系ガス、臭素系ガス等のハロゲン系ガスは、単独で用いることもできるし、２種類以上を混合して用いることもできる。 Halogenous gases such as the chlorine-based gas, fluorine-based gas, and bromine-based gas can be used alone or in combination of two or more.
本発明では、上記硬質皮膜コーティングが施された金属部材を、ハロゲン系ガスが存在する雰囲気中において加熱保持する。この加熱保持により、表面の硬質皮膜コーティングをハロゲン化物とすることにより除去することが行われる。 In the present invention, the metal member to which the hard film coating is applied is heated and held in an atmosphere in which a halogen-based gas exists. By this heating and holding, the surface hard film coating is removed by using a halide.
上記加熱保持の際の圧力は大気圧近傍とすることができる。大気圧近傍で加熱保持するときは、所定温度に加熱した炉内に処理対象の金属部材を装入し、炉内圧力を大気圧近傍に保持しながら炉内にハロゲン系ガスを導入してパージし、さらに所定時間保持することが行われる。このとき炉内に導入されるハロゲン系ガスは、主成分ガスを希釈ガスで希釈したガスを導入することがおこなわれる。ここで、上記大気圧近傍の圧力とは、−２００Ｐａ〜２００Ｐａの範囲内の圧力をいう。 The pressure at the time of heating and holding can be close to atmospheric pressure. When heating and holding near atmospheric pressure, a metal member to be treated is placed in a furnace heated to a predetermined temperature, and purged by introducing a halogen-based gas into the furnace while maintaining the furnace pressure near atmospheric pressure. Further, holding for a predetermined time is performed. At this time, as the halogen-based gas introduced into the furnace, a gas obtained by diluting the main component gas with a diluent gas is introduced. Here, the pressure in the vicinity of the atmospheric pressure refers to a pressure within a range of −200 Pa to 200 Pa.
希釈ガスで希釈されたハロゲン系ガス中の主成分ガスの濃度は、２容量％以上２０容量％以下程度が好ましい。２容量％未満では硬質皮膜コーティングを除去するのに時間を要してしまい、２０容量％を超えてもそれほどの時間短縮や効率アップが望めないからである。 The concentration of the main component gas in the halogen-based gas diluted with the dilution gas is preferably about 2% by volume or more and 20% by volume or less. This is because if it is less than 2% by volume, it takes time to remove the hard coating, and if it exceeds 20% by volume, it is not possible to reduce the time and increase efficiency.
また、加熱保持の際の圧力は、減圧雰囲気とすることもできる。減圧雰囲気で加熱保持するときは、所定温度に加熱した炉内に処理対象の金属部材を装入し、炉内を真空ポンプで減圧したのち炉内にハロゲン系ガスを導入し、さらに所定時間保持することが行われる。このとき炉内に導入されるハロゲン系ガスは、主成分ガスを希釈ガスで希釈しないか、主成分ガスの濃度を２容量％以上としたガスを導入することがおこなわれる。ここで、上記減圧雰囲気の圧力は、上記大気圧近傍圧力未満で１ｋＰａまでの範囲内の圧力である。 Moreover, the pressure at the time of heating and holding can be a reduced pressure atmosphere. When heating and holding in a reduced pressure atmosphere, the metal member to be treated is placed in a furnace heated to a predetermined temperature, the pressure in the furnace is reduced by a vacuum pump, a halogen-based gas is introduced into the furnace, and the holding is continued for a predetermined time. To be done. At this time, as the halogen-based gas introduced into the furnace, the main component gas is not diluted with a diluent gas, or a gas in which the concentration of the main component gas is 2% by volume or more is introduced. Here, the pressure of the reduced pressure atmosphere is a pressure within a range of less than the atmospheric pressure and up to 1 kPa.
このように、上記加熱保持は、金属部材をプラズマ中に晒さないで行う。このため、プラズマ発生装置等の設備のない雰囲気炉により処理が可能となるため、設備の兼用や流用が容易であり、コストを大幅に節減することができる。 Thus, the heating and holding is performed without exposing the metal member to plasma. For this reason, since it becomes possible to perform processing in an atmospheric furnace without equipment such as a plasma generator, it is easy to share and divert equipment, and the cost can be greatly reduced.
また、上記加熱保持の温度は１００℃を超え５００℃以下とするのが好ましい。１００℃以下であると硬質皮膜コーティングを除去するのに時間を要し、５００℃を超えてもそれほどの時間短縮や処理効率の向上を望めないうえ、高温保持による母材の軟化が生じるおそれがあるからである。 The heating and holding temperature is preferably more than 100 ° C. and 500 ° C. or less. If it is 100 ° C. or lower, it takes time to remove the hard coating, and even if it exceeds 500 ° C., it cannot be expected to shorten the time or improve the processing efficiency, and the base material may be softened by holding at a high temperature. Because there is.
ハロゲン系ガスとして塩素系ガスを使用した場合は、上記加熱保持の温度を、１００〜４００℃℃とするのが好ましい。また、上記ハロゲン系ガスとして塩素系ガス以外のハロゲン系ガスを使用した場合は、上記加熱保持の温度を、１５０〜５００℃とするのが好ましい。 When a chlorine-based gas is used as the halogen-based gas, the heating and holding temperature is preferably 100 to 400 ° C. Moreover, when halogen-type gas other than chlorine-type gas is used as said halogen-type gas, it is preferable that the temperature of the said heating holding shall be 150-500 degreeC.
上記加熱保持の時間は、１５分以上とするのが好ましい。１５分未満では、硬質皮膜コーティングの除去が十分行われないおそれがあるからである。加熱保持時間は長いほうが硬質皮膜コーティングの除去が進むのであるが、硬質皮膜コーティングが除去されているのに加熱し続けても意味がない。したがって加熱時間は、１５分を下限とし、硬質皮膜コーティングの種類、厚み、ハロゲン系ガスの濃度、加熱温度等の諸条件に応じて適宜決定されるが、おおむね最大６時間程度まで、通常は２〜３時間程度までで終了する。 The heating and holding time is preferably 15 minutes or longer. This is because if it is less than 15 minutes, the hard coating may not be sufficiently removed. The longer the heating and holding time, the more the hard film coating is removed, but there is no point in continuing to heat even though the hard film coating has been removed. Therefore, the heating time is 15 minutes as a lower limit, and is appropriately determined according to various conditions such as the type of hard coating, thickness, halogen-based gas concentration, heating temperature, etc., but is generally up to about 6 hours, usually 2 It ends in about 3 hours.
このように、硬質皮膜コーティングが施された金属部材をハロゲン系ガスが存在する雰囲気中で加熱保持し、表面の硬質皮膜コーティングをハロゲン化物とすることにより除去する。 As described above, the metal member to which the hard film coating is applied is heated and held in an atmosphere in which a halogen-based gas exists, and the hard film coating on the surface is removed by using a halide.
一例をあげると、例えば、ＴｉＮコーティングをＮＦ３ガス雰囲気中に加熱保持すると、下記の式（１）に示すようにＴｉＦ４が生成する。ＴｉＦ４は蒸気圧が高いため、生成されるとほぼ同時に蒸発する。このようにして、母材表面からＴｉＮコーティングが除去される。
６ＴｉＮ＋８ＮＦ３→６ＴｉＦ４＋７Ｎ２…（１）
For example, when the TiN coating is heated and held in an NF 3 gas atmosphere, TiF 4 is generated as shown in the following formula (1). Since TiF 4 has a high vapor pressure, it evaporates almost simultaneously when produced. In this way, the TiN coating is removed from the surface of the base material.
6TiN + 8NF 3 → 6TiF 4 + 7N 2 (1)
また、ＣｒＮコーティングをＮＦ３ガス雰囲気中に加熱保持すると、下記の式（２）に示すようにＣｒＦ３が生成する。ＣｒＦ３は脆くて弱いため、生成されるとパラパラと表面から剥離する。このようにして、母材表面からＣｒＮコーティングが除去される。
ＣｒＮ＋ＮＦ３→ＣｒＦ３＋Ｎ２…（２）
When the CrN coating is heated and held in an NF 3 gas atmosphere, CrF 3 is generated as shown in the following formula (2). Since CrF 3 is brittle and weak, when it is formed, it peels off from the surface. In this way, the CrN coating is removed from the base material surface.
CrN + NF 3 → CrF 3 + N 2 (2)
このように硬質皮膜コーティングを除去した後は、必要に応じて再研磨処理、再コーティング処理を行い、工具類や機械部品として再生する。 After removing the hard coating as described above, re-polishing and re-coating are performed as necessary, and the hard coating is regenerated as tools and machine parts.
つぎに、実施例について説明する。 Next, examples will be described.
〔実施例１〕
＜試験材１＞：ダイス用超硬合金（ＷＣ；９０重量％、Ｃｏ；１０重量％）ＪＩＳ Ｖ３０相当の金型表面にイオンプレーティング法により膜厚２μｍのＴｉＮ皮膜を形成した。
この試験材１を、１０容量％ＮＦ３、９０容量％Ｎ２雰囲気の炉内において２４０℃×３０分間処理し、超硬合金金型表面からＴｉＮ皮膜を剥離・除去した。
[Example 1]
<
This
〔実施例２〕
＜試験材２＞：超硬合金（ＷＣ；７１重量％、ＴｉＣ；９重量％、ＴｉＮ；０．５重量％、ＴａＣ；１０重量％、Ｃｏ；９．５重量％）ＪＩＳ Ｐ３０相当のスローアウェイチップ表面にＣＶＤ法により膜厚３μｍのＴｉＮ−ＴｉＣＮ皮膜を形成した。
この試験材２を、５容量％ＮＦ３、９５容量％Ｎ２雰囲気の炉内において３００℃×６０分間処理し、超硬合金金型表面からＴｉＮ−ＴｉＣＮ皮膜を剥離・除去した。
[Example 2]
<Test material 2>: Cemented carbide (WC; 71 wt%, TiC; 9 wt%, TiN; 0.5 wt%, TaC; 10 wt%, Co; 9.5 wt%) JIS P30 equivalent throwaway A TiN—TiCN film having a thickness of 3 μm was formed on the chip surface by CVD.
This test material 2 was treated at 300 ° C. for 60 minutes in a 5 vol% NF 3 , 95 vol% N 2 atmosphere furnace to peel and remove the TiN—TiCN film from the cemented carbide mold surface.
〔実施例３〕
＜試験材３＞：ダイス用超硬合金（ＷＣ；８５重量％、Ｃｏ；１５重量％）ＪＩＳ Ｖ５０相当の金型表面にイオンプレーティング法により膜厚２μｍのＴｉＮ−ＴｉＳｉＮ皮膜を形成した。
この試験材３を、１０容量％ＮＦ３、９０容量％Ｎ２雰囲気の炉内において３５０℃×９０分間処理し、超硬合金金型表面からＴｉＮ−ＴｉＳｉＮ皮膜を剥離・除去した。
Example 3
<Test Material 3>: Cemented carbide for dies (WC; 85% by weight, Co; 15% by weight) A TiN—TiSiN film having a thickness of 2 μm was formed on the die surface corresponding to JIS V50 by an ion plating method.
This test material 3 was treated at 350 ° C. for 90 minutes in a furnace of 10 volume% NF 3 and 90 volume% N 2 atmosphere to peel and remove the TiN—TiSiN film from the surface of the cemented carbide mold.
〔実施例４〕
＜試験材４＞：切削工具用超硬合金（ＷＣ；９０重量％、Ｃｏ；１０重量％）ＪＩＳ Ｋ２０相当のリーマ表面にイオンプレーティング法により膜厚２μｍのＴｉＡｌＮ皮膜を形成した。
この試験材４を、１０容量％ＮＦ３、９０容量％Ｎ２雰囲気の炉内において３５０℃×９０分間処理し、超硬合金金型表面からＴｉＡｌＮ皮膜を剥離・除去した。
Example 4
<Test Material 4>: Cemented carbide for cutting tools (WC; 90% by weight, Co; 10% by weight) A TiAlN film having a thickness of 2 μm was formed on the surface of a reamer equivalent to JIS K20 by an ion plating method.
This test material 4 was treated in a furnace of 10 volume% NF 3 and 90 volume% N 2 atmosphere at 350 ° C. for 90 minutes to peel and remove the TiAlN coating from the cemented carbide mold surface.
〔実施例５〕
上記試験材１の成膜試料を新品膜としてスクラッチ試験に供した。一方、上記試験材１の成膜試料を、１０容量％ＮＦ３、９０容量％Ｎ２雰囲気の炉内において２４０℃×３０分間処理し、超硬合金金型表面からＴｉＮ皮膜を剥離・除去した。その後、全く同一の成膜条件でＴｉＮを再コーティングし、スクラッチ試験に供した。
Example 5
The film formation sample of the
スクラッチ試験は、ナノテック社製ＣＳＥＭ ＲＥＶＥＴＥＳＴスクラッチ試験機を用いた。試験結果を図１に示す。図１からわかるように、膜剥離の臨界荷重Ｌｃ値の測定結果は両者とも７５Ｎであり、除膜再コーティングの場合でも膜の密着性は新品と同様であることがわかった。 For the scratch test, a CSEM REVETEST scratch tester manufactured by Nanotech Co., Ltd. was used. The test results are shown in FIG. As can be seen from FIG. 1, the measurement results of the critical load Lc value for film peeling were both 75 N, and it was found that even in the case of film removal recoating, the adhesion of the film was the same as that of a new product.
〔比較例１〕
上記試験材１，２，３について、３５％溶液の過酸化水素水−ニトロ化合物−アンモニア水−アミン化合物で形成された市販の剥離液に、２２℃で２０時間浸漬した。
[Comparative Example 1]
The
〔比較例２〕
上記試験材４について、剥離剤３５％溶液の過酸化水素水−アンモニア水−アミン化合物で形成された市販の剥離液に、２０℃で４８時間浸漬した。
[Comparative Example 2]
About the said test material 4, it immersed in the commercially available peeling liquid formed with the hydrogen peroxide water-ammonia water-amine compound of 35% of release agent at 20 degreeC for 48 hours.
〔比較例３〕
上記試験材１について、剥離剤３５％溶液の過酸化水素水−水酸化ナトリウム−ＥＤＴＡ等で形成された市販の剥離液に、２０℃で１４時間浸漬した。
[Comparative Example 3]
About the said
上記各実施例および比較例について、硬質皮膜のコーティング前と皮膜除去後について表面粗さを測定した結果を下記の表１に示す。表１から明らかなように、比較例に比べて実施例については皮膜除去後の表面粗さが小さいレベルにあることがわかる。 Table 1 below shows the results of measuring the surface roughness of each of the above Examples and Comparative Examples before and after removing the hard film. As is clear from Table 1, it can be seen that the surface roughness after removal of the film is at a level that is smaller than that of the comparative example.
以上のように、本発明は、従来の薬液処理に比べて大幅に短い時間で硬質皮膜コーティングを除去し、工具または金型の再生を行うことができる。そして、硬質皮膜コーティングが除去された工具または金型は、必要に応じて再研磨を行い、再コーティングを行って再利用することができる。また、本発明の硬質皮膜コーティングされた工具または金型の再生方法は、従来のようにプラズマ雰囲気ではなく、加熱雰囲気を利用するため、高価な設備が不要で極めて安価に再生処理を行うことができる。さらに、母材が超硬合金であっても従来の薬液処理のようにＣｏ溶出による母材の損傷や粗れが生じないため、再生後の金属部品の耐磨耗性等に悪影響を及ぼさない。
As described above, the onset Ming can the hard film coating is removed in a much shorter time compared to conventional chemical treatment, to reproduce tool or mold. The tool or die hard film coating has been removed, have rows regrinding optionally, can be reused by performing recoat. In addition, the method for regenerating a hard film coated tool or mold according to the present invention uses a heating atmosphere instead of a plasma atmosphere as in the prior art, so that expensive equipment is not required and the regeneration process can be performed at a very low cost. it can. Furthermore, even if the base material is a cemented carbide, the base material is not damaged or roughened due to Co elution unlike the conventional chemical treatment, so it does not adversely affect the wear resistance of the metal parts after recycling. .
また、上記加熱保持は工具または金型をプラズマ中に晒さないで行う場合には、高価なプラズマ発生設備が不要で、極めて安価に再生処理を行うことができる。
In addition, when the heating and holding are performed without exposing the tool or the mold to the plasma, an expensive plasma generating facility is unnecessary, and the regeneration process can be performed at a very low cost.
また、上記加熱保持の温度は２００℃を超え４００℃以下である場合には、硬質皮膜コーティングを十分に除去することができ、かつ不必要に高温保持することによる母材の軟化等を防止する。
Further, when the temperature of the heating and holding is more than 200 ° C. and not more than 400 ° C., the hard film coating can be sufficiently removed, and the base material is softened by holding at an unnecessarily high temperature. To prevent.
また、上記加熱保持の時間は３０分以上である場合には、硬質皮膜コーティングを十分に除去することができる。
Further, when the heating and holding time is 30 minutes or longer, the hard coating can be sufficiently removed.
また、上記加熱保持の際の圧力は大気圧近傍である場合には、大気圧の加熱炉内をハロゲン系ガスでパージして加熱保持すればよいことから、容易かつ安価に再生処理を行うことができる。 In addition, when the pressure at the time of the heating and holding is near atmospheric pressure, the inside of the atmospheric heating furnace may be purged with a halogen-based gas and heated and held, so that the regeneration process can be performed easily and inexpensively. Can do.
また、上記ハロゲン系ガスがＮＦ３系ガスである場合には、反応性、取り扱い性等の面で優れており、実用的である。 In addition, when the halogen-based gas is an NF 3 -based gas, it is excellent in terms of reactivity, handleability, etc., and is practical.
Claims (6)
上記加熱した雰囲気炉内に、主成分ガスに希釈ガスを加えたプラズマを含まないハロゲン系化合物ガスを導入して上記ハロゲン系化合物ガスが存在する大気圧近傍の雰囲気中において工具を加熱保持し、
上記工具をプラズマ中に晒さないで、プラズマを含まないハロゲン系化合物ガスにより表面の硬質皮膜コーティングをハロゲン化物とすることにより除去し、
その後、硬質皮膜コーティングの再コーティング処理を行うことを特徴とする硬質皮膜コーティングされた工具の再生方法。 The tool hard film coating is applied by PVD or CVD, and heated in an atmosphere furnace without plasma generation equipment,
Into the heated atmospheric furnace, a halogen-based compound gas not containing a plasma in which a diluent gas is added to the main component gas is introduced to heat and hold the tool in an atmosphere near the atmospheric pressure where the halogen-based compound gas exists,
Without exposing the above tool to the plasma, removing the hard film coating on the surface with a halogen-based compound gas that does not contain plasma to remove it,
Thereafter, a hard film-coated tool is regenerated by performing a re-coating process of the hard film coating.
上記加熱した雰囲気炉内に、主成分ガスに希釈ガスを加えたプラズマを含まないハロゲン系化合物ガスを導入して上記ハロゲン系化合物ガスが存在する大気圧近傍の雰囲気中において金型を加熱保持し、
上記金型をプラズマ中に晒さないで、プラズマを含まないハロゲン系化合物ガスにより表面の硬質皮膜コーティングをハロゲン化物とすることにより除去し、
その後、硬質皮膜コーティングの再コーティング処理を行うことを特徴とする硬質皮膜コーティングされた金型の再生方法。 A mold hard film coating is applied by PVD or CVD, and heated in an atmosphere furnace without plasma generation equipment,
Into the heated atmosphere furnace, a halogen-based compound gas not containing plasma in which a diluent gas is added to the main component gas is introduced, and the mold is heated and maintained in an atmosphere near the atmospheric pressure where the halogen-based compound gas exists. ,
Without exposing the above mold to the plasma, removing the hard film coating on the surface with a halogen-based compound gas that does not contain plasma to remove it,
Thereafter, a hard film-coated mold is regenerated by performing a re-coating process of the hard film coating.
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