WO2009104273A1 - Produit en alliage base fer avec revêtement composite - Google Patents

Produit en alliage base fer avec revêtement composite Download PDF

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Publication number
WO2009104273A1
WO2009104273A1 PCT/JP2008/053063 JP2008053063W WO2009104273A1 WO 2009104273 A1 WO2009104273 A1 WO 2009104273A1 JP 2008053063 W JP2008053063 W JP 2008053063W WO 2009104273 A1 WO2009104273 A1 WO 2009104273A1
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WO
WIPO (PCT)
Prior art keywords
film
iron
composite coating
alloy product
gas
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PCT/JP2008/053063
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English (en)
Japanese (ja)
Inventor
井原仁史
佐藤嘉高
渡部清彦
丹羽司
Original Assignee
ユケン工業株式会社
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Application filed by ユケン工業株式会社 filed Critical ユケン工業株式会社
Priority to PCT/JP2008/053063 priority Critical patent/WO2009104273A1/fr
Publication of WO2009104273A1 publication Critical patent/WO2009104273A1/fr

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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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0635—Carbides
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating

Definitions

  • the present invention relates to an iron-based alloy product provided with a composite coating.
  • a composite coating is removed after use over time, and a composite coating is formed again by new ion plating (hereinafter referred to as “IP”).
  • IP new ion plating
  • a metal plastic working die (press die) will be described as an example of an iron-based alloy product.
  • the present invention is not limited to this and is applicable to other cutting tools and resin molding dies. Is possible.
  • metal plastic working molds such as press molds are generally made of an iron-based alloy (steel), so that it is necessary to perform a composite coating treatment in order to maintain durability such as wear resistance. .
  • steel iron-based alloy
  • One of the composite coating processes is vanadium carbide (VC) film processing.
  • VC vanadium carbide
  • the main method for forming a VC film is a thermal reaction precipitation diffusion method (TRD method: Thermal Reactive Deposition and Diffusion) (see Patent Documents 1, 2, and 3).
  • the bath temperature it is necessary to set the bath temperature to 800 to 1200 ° C. (see the above publication), which is not desirable from the viewpoint of working environment, energy saving, productivity, and the like. That is, the working environment became high temperature, energy for maintaining the bath temperature was required, and it took time to cool the product after coating.
  • Patent Document 4 a method for forming a vanadium-based film (composite film) having the following configuration, and obtained a patent having the following configuration (Patent Document 4).
  • the vanadium-based coating is a composite coating composed of a VN film, a VCN film, and a VC film sequentially arranged from the substrate side, Each layer of the vanadium-based coating is formed by reaction by using vanadium as an evaporation source and adjusting and maintaining the injection gas amount and gas ratio corresponding to the film type using nitrogen gas and / or hydrocarbon gas as the injection gas.
  • a method for forming a vanadium-based film characterized by the above.
  • the composite coating (vanadium-based coating) is worn out after a long period of use (for example, the number of presses of 100,000 to 150,000), and a predetermined molded product ( It is difficult to ensure the processing accuracy of plastic processed products.
  • the composite coating is dissolved and removed using a solution for the constituent metal of the composite coating.
  • the present invention has a small surface roughness of the iron-based alloy substrate (mold body) after removing the composite coating with a metal solution, and requires little smoothing such as grinding or lapping. It is an object (problem) to provide an iron-based alloy material capable of forming a new composite film.
  • the present inventors made the composite coating into the following film configuration, thereby dissolving the hard composite film with a general-purpose (commercially available) titanium-based metal solution. It was found that the surface roughness of the iron-based substrate after dissolution and removal was small, and a new composite film could be formed without substantial grinding or lapping.
  • an iron-based alloy product comprising a vanadium (V) -based / titanium (Ti) -based hard composite coating on the surface of an iron-based alloy substrate containing chromium carbide
  • the hard composite coating includes a TiN film, a TiVCN film, and a VC film sequentially arranged from the substrate side, and the VC film is located on the outermost surface.
  • the present inventors can dissolve and remove it with a commercially available release agent for titanium-based IP (dissolution solution), as shown in Examples described later, I found out. That is, the speed of dissolving the VC film of the titanium-based IP release agent is slower than that of the Ti-based film, but when a large number of pinholes appear in the second-layer TiVCN film due to slight dissolution of the VC film, The lower layer TiN is dissolved first, and the composite film is peeled and removed in the film state.
  • a commercially available release agent for titanium-based IP dissolution solution
  • the number of pretreatment steps such as grinding and lapping of the mold surface for reducing the surface roughness can be substantially reduced.
  • the iron-base alloy base material is not particularly limited as long as it is a steel material containing chromium, chromium carbide is generated to some extent. Usually, it is selected from the group of steel materials having a chromium content of 1.0 to 30% by mass, preferably 5.0 to 25% by mass (see Table 1).
  • the iron-based alloy product having each of the above-described structures is formed on the surface of the iron-based alloy base material using V and / or Ti as an evaporation source and nitrogen gas and / or hydrocarbon gas as an injection gas amount / gas ratio. Can be adjusted and maintained in accordance with the film type, whereby each layer of the composite coating can be produced by reaction film formation.
  • the composition of the film formation is good from the composition having good adhesion to the iron-based alloy substrate (normally low hardness) to the composition having good wear resistance (normally high hardness). It can be changed stepwise or continuously.
  • the substrate temperature during film formation is usually adjusted in the range of 400 to 500 ° C.
  • the tempering temperature of the tough steel is usually about 500 to 650 ° C. Therefore, when temperature variation is taken into consideration, 500 ° C. or less is desirable. It becomes difficult to get sex.
  • the upper limit of the IP film formation temperature (substrate temperature) is usually 550 ° C.
  • Model diagram showing an example of a composite coating in the present invention Schematic model diagram showing an example of an IP device used in the present invention
  • TiN, TiVCN, and VC mean vanadium nitride (cubic system), titanium vanadium carbonitride (same), and vanadium carbide (same), respectively.
  • HV Vickers hardness measured according to JIS Z 2244.
  • FIG. 1 is a partial cross-sectional view of an iron-based alloy product according to an embodiment of the present invention.
  • a TiN film 14 and a TiVCN are arranged on the surface of a steel base 12 in order from the base 12 side.
  • This is an iron-based alloy product (for example, a mold for plastic working) provided with a vanadium-based composite coating composed of the film 16 and the VC film 18.
  • the TiN film 14, the TiVCN film 16, and the VC film 18 are arranged in this order from the base material 12 side, the hardness increases in that order as described above, and the base material, particularly a steel base material (usually HV 600 to 900). And the hardness difference can be reduced. Therefore, even if the surface hardness is high, it becomes easy to ensure adhesion with the substrate.
  • the VC film 18 is HV3500, and it is easy to ensure the surface hardness that is a factor (parameter) for ensuring wear resistance. If further improvement in wear resistance is required, it is desirable to reduce the friction coefficient (dynamic friction coefficient: JIS K 7125), which is another factor of wear resistance.
  • the dynamic friction coefficient ( ⁇ ) is 0.3 or less, preferably 0.2 or less. As will be described later, the friction coefficient can be easily obtained by increasing the amount of hydrocarbon (carbon source).
  • first and second interlayer coupling layers 20 and 22 having a gradient composition are further interposed between the layers of the composite coating, that is, between the TiN film 14 / TiVCN film 16 / VC film 18. I'm allowed. That is, the first interlayer coupling layer 20 is a Ti-rich TiVCN graded layer, and the second interlayer coupling layer 22 is a V-rich TiVCN graded layer.
  • TiVCN layer to the TiVCN gradient layer are considered to exist mostly in the form of TiVCN compounds, but are also considered to exist somewhat in the form of other polyvalent compounds of TiC, TiN, TiCN, VC, VN and VCN.
  • interlayer bonding layers 20 and 22 further reduces the hardness difference between the respective layers, and as a result, delamination due to mechanical shock or thermal shock hardly occurs, and as a result, the toughness of the vanadium-based coating increases. That is, durability is increased.
  • the thickness is 8 to 2.5 / 2.5 / 5, most preferably about 2/2/6, and the total film thickness is 2 to 50 ⁇ m, preferably 3 to 12 ⁇ m, and most preferably about 10 ⁇ m.
  • the film thickness ratio of the VC film to the TiN film or the TiVCN film is too large, the compression stress of the film increases when the film thickness of the VC film exceeds 10 ⁇ m. Delamination with the TiVCN film is likely to occur. Moreover, since the film toughness is lowered, cracks are likely to occur in the VC film due to impact during forging.
  • the film thickness ratio of the VC film to the TiN film or TiVCN film is too small, the hardness of the entire coating becomes HV3300 or less, making it difficult to obtain wear resistance.
  • the layer thickness (film thickness) of the interlayer coupling layers 20 and 22 is much thinner than the TiN film, the TiVCN film, and the VC film that are the constituent layers of the vanadium-based film. It is desirable that the layer be as thin as possible if it has an interlayer coupling effect. Usually, it is 0.5 / 10 to 3/10, preferably 1/10 to 2/10, most preferably TiN film or TiVCN film. About 1.5 / 10. The reason for the setting is estimated as follows.
  • the iron-based alloy a steel material (usually tool steel) having a chromium content of 1.0 to 30% by mass is used.
  • the steel material not containing chromium according to the present invention does not have the problem of solving the problem of the present invention (the mold surface after the removal of the composite film becomes a fluttered surface), and is mechanically similar to a metal plastic working mold. This is because iron-base alloy products that are susceptible to shock and thermal shock are planned.
  • Fe-based alloys such as high-speed steel, die steel, powdered high-speed steel, and semi-high-speed steel can be suitably used.
  • iron-based alloy examples include those shown in Table 1.
  • Table 1 the chromium content of each steel material is also shown.
  • the iron base alloy product (mold for plastic working) of the above embodiment will be described by taking as an example a case where a composite film is formed (film formation) on an iron base alloy substrate made of tool steel. do.
  • an IP device as shown in FIG. 2 usually an arc IP (AIP) device, is used.
  • the AIP method uses vanadium as an evaporation source, nitrogen gas and / or hydrocarbon gas as a source gas, and adjusts and maintains the injection gas amount and gas ratio corresponding to the film type, thereby forming a TiN film, a TiVCN film, and a VC film. This is because it is easy to form a reactive film on a substrate with high purity.
  • IP methods such as a multi-cathode thermionic irradiation method, a high-frequency excitation method, a holo-cathode discharge method, a cluster method, and an activated reaction deposition method are also possible.
  • the IP device includes a plurality of (two in the illustrated example) evaporation source holding portions (pot portions) 25 and 25A for holding titanium or vanadium in a chamber 24, and a workpiece (base) connected to a bias voltage source 26. Material) 28 is provided. Furthermore, the chamber 24 includes an exhaust port 32 connected to an exhaust pump that maintains the inside of the chamber at a predetermined degree of vacuum, and a reaction gas introduction port 34 for introducing a reaction gas (nitrogen and / or methane). A heater 36 that maintains the interior at a predetermined temperature and also maintains the substrate (substrate) 28 at a predetermined temperature is provided.
  • titanium (Ti) and vanadium (V) are usually used in a purity of tunaine to threeine.
  • the gas that is the source of nitrogen and carbon, which are elements that react with vanadium can use nitrogen gas (N 2 ) for the former and hydrocarbon gases such as methane (CH 4 ), ethane, ethylene, acetylene for the latter It is.
  • N 2 nitrogen gas
  • hydrocarbon gases such as methane (CH 4 ), ethane, ethylene, acetylene for the latter It is.
  • methane which is difficult to generate soot, is desirable because unreactive gas contaminates the surface of the apparatus and the substrate.
  • the purity of each is made from three nine to six nine.
  • the film formation conditions by the AIP method are as shown in Table 2, for example.
  • one or both pots holding titanium and vanadium are heated, and one or both of them are dissolved and evaporated simultaneously.
  • titanium is first held in all pots, heated and evaporated to form the first layer (TiN film), the vacuum in the chamber is released, and half of the plurality of pots are replaced, and the second A layer (TiVCN film) and a third layer (VC film) can also be sequentially formed.
  • Degree of vacuum If the degree of vacuum is too high (the absolute pressure is low), the amount of reaction gas will be small, the deposition rate will be slowed and productivity will be reduced, and the deposited film will contain excessive metal components. Or the particles are coarse and have many voids. (It is estimated that the generation of crystal nuclei is delayed.) On the other hand, if the degree of vacuum is too low (the absolute pressure is high), the amount of reaction gas becomes excessive, and the gas that is not used in the reaction and not fully activated acts as an adsorption inhibitor (inhibitor) on the growth film surface. There is a risk.
  • the surface film when application of the present invention to a mold is expected to improve wear resistance, the surface film (VC film) is required to have slipperiness as well as film hardness. In such a case, it acts as a lubricant. It is desirable to contain C (carbon) in the film. However, when the C content is excessive, the film hardness is lowered and the wear resistance is also lowered.
  • the degree of vacuum that can achieve such a balance is about 10 to 50 mtorr (1.33 to 6.65 Pa), preferably about 20 mtorr (2.66 Pa), and the amount of methane gas is about 400 to 600 mL / min, preferably about 500 mL / min.
  • Arc current If the current value is too low, the film forming speed is slow, and conversely if it is too high, it is not desirable from the viewpoint of the safety of the apparatus.
  • Bias voltage Generally, the higher the bias voltage, the slower the film formation speed. Therefore, the bias voltage is set within an appropriate range in consideration of productivity.
  • the supply gas is nitrogen (N 2 )
  • nitrogen (N 2 ) there is almost no influence on the nitride film crystal of the bias voltage, and it can be appropriately set within the range of 50 to 400V, preferably 50 to 200V.
  • a hydrocarbon such as CH 4
  • the bias voltage is low, the crystallinity of VC becomes low and it becomes difficult to obtain the wear resistance of the carbide film. Therefore, like nitrogen, it can be in the range of 50 to 400 V, but is preferably about 100 to 200 V, and more preferably about 150 V, from the balance between productivity and crystallinity.
  • Substrate temperature The higher the temperature, the faster the film formation rate is desirable, but from the standpoint of energy saving and heat resistance of the base material, when the base material is steel, the temperature is below the temperature at which dimensional distortion due to tempering does not occur, usually 350 ⁇ 550 ° C., preferably 400 to 500 ° C. In the case where the substrate does not generate thermal strain as in the case of ceramics, it may be performed at a maximum IP temperature of about 550 ° C.
  • Table 3 shows an example of the gas flow rate and the deposition time when an interlayer coupling layer is formed between the layers.
  • the amount and pressure of the gas in each interlayer bonding layer in Table 2 do not instantaneously become the amount and pressure, but usually increase continuously to the pressure after an intermediate time of the film formation time, for example, 40 to 50 s, Thereafter, the set value is maintained.
  • the lower hardness is the base material side, and an interlayer coupling layer is formed between each layer.
  • the TiN film having the lowest hardness has a hardness of HV2000, and preferably a vanadium-based film having a hardness of HV3000 or more is easily formed on a substrate such as steel with good adhesion. it can.
  • IP4024 type manufactured by Kobe Steel Co., Ltd. was used as the IP device.
  • V was filled with 800 g of pure three nine
  • N 2 was pure five nine
  • CH 4 was pure three nine.
  • a press die made of cold die steel (SKD11: HV650, HRC58.0) was used as the film forming substrate.
  • the shape of the mold was a short square column, and before forming the composite coating, a length: 70.200 mm, a width: 55.900 mm, and a height: 42.000 mm were used.
  • Example: In Table 3, a composite film (TiN film / TiVCN film / VC film) having a total film thickness of about 10 ⁇ m was formed on the press surface (molded surface) of the mold as a base material with X 1200 s.
  • a composite coating (TiN film / TiVCN film / VC film) having a total film thickness of about 10 ⁇ m was formed on the press surface of a mold as a base material under the film forming conditions shown in Table 4.
  • Vanadium-based IP release agent acidic aqueous solution
  • the conditions were 30 ° C. ⁇ 12 h.
  • the length was ⁇ 90 ⁇ m and the height was ⁇ 120 ⁇ m, whereas in the example, the length was ⁇ 1 ⁇ mm and the height was ⁇ 2 ⁇ m. That is, in the present invention, it was confirmed that the wrapping amount may be very small.

Abstract

La présente invention concerne un produit en alliage base fer, tel qu'un moule métallique pour la mise en forme de plastique, ayant un revêtement composite à base de vanadium (V) superposé sur un substrat en alliage base fer contenant du chrome (12). Le revêtement composite est composé, par superposition séquentielle en partant du substrat, d'un film de TiN (14), d'un film de TiVCN (16) et d'un film de VC (18). Le revêtement composite est formé en plaçant d'abord un substrat en alliage base fer dans une chambre d'un appareil de placage ionique et en effectuant une rétention de régulation du rapport taux de gaz injecté/gaz en correspondance avec les espèces de film tout en utilisant du titane et/ou du vanadium comme source d'évaporation et en utilisant de l'azote et/ou de l'hydrocarbure gazeux comme gaz injecté pour ainsi obtenir la formation d'un film de réaction pour chacune des couches individuelles. Ce produit en alliage base fer présente une faible rugosité de surface du substrat en alliage base fer (corps principal du moule métallique) après élimination du revêtement composite par un liquide de dissolution du métal, permettant ainsi la formation d'un nouveau revêtement composite presque sans opérations de meulage et de polissage.
PCT/JP2008/053063 2008-02-22 2008-02-22 Produit en alliage base fer avec revêtement composite WO2009104273A1 (fr)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012158793A (ja) * 2011-01-31 2012-08-23 Tottori Institute Of Industrial Technology 成膜方法及び硬質被膜被覆部材
CN105102664A (zh) * 2013-03-29 2015-11-25 西铁城控股株式会社 具有灰色色调层的硬质装饰构件
CN114872311A (zh) * 2021-02-05 2022-08-09 苏州泛普智能科技有限公司 自动覆膜装置

Citations (5)

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JPH10237628A (ja) * 1997-02-20 1998-09-08 Sumitomo Electric Ind Ltd 被覆工具およびその製造方法
JP2000107906A (ja) * 1998-10-05 2000-04-18 Hitachi Tool Engineering Ltd 被覆硬質工具
JP2000271699A (ja) * 1999-03-23 2000-10-03 Sumitomo Electric Ind Ltd 表面被覆成形型およびその製造方法
JP2002371352A (ja) * 2001-06-15 2002-12-26 Yuken Industry Co Ltd バナジウム系被膜の成膜方法
JP2005046975A (ja) * 2003-07-31 2005-02-24 Nachi Fujikoshi Corp バナジウム系被覆工具

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10237628A (ja) * 1997-02-20 1998-09-08 Sumitomo Electric Ind Ltd 被覆工具およびその製造方法
JP2000107906A (ja) * 1998-10-05 2000-04-18 Hitachi Tool Engineering Ltd 被覆硬質工具
JP2000271699A (ja) * 1999-03-23 2000-10-03 Sumitomo Electric Ind Ltd 表面被覆成形型およびその製造方法
JP2002371352A (ja) * 2001-06-15 2002-12-26 Yuken Industry Co Ltd バナジウム系被膜の成膜方法
JP2005046975A (ja) * 2003-07-31 2005-02-24 Nachi Fujikoshi Corp バナジウム系被覆工具

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012158793A (ja) * 2011-01-31 2012-08-23 Tottori Institute Of Industrial Technology 成膜方法及び硬質被膜被覆部材
CN105102664A (zh) * 2013-03-29 2015-11-25 西铁城控股株式会社 具有灰色色调层的硬质装饰构件
US20160053360A1 (en) * 2013-03-29 2016-02-25 Citizen Watch Co., Ltd. Hard decorative member having gray-tone layer
EP2980264A4 (fr) * 2013-03-29 2016-12-28 Citizen Holdings Co Ltd Composant décoratif rigide ayant une couche de ton gris
US9869011B2 (en) 2013-03-29 2018-01-16 Citizen Watch Co., Ltd. Hard decorative member having gray-tone layer
CN114872311A (zh) * 2021-02-05 2022-08-09 苏州泛普智能科技有限公司 自动覆膜装置
CN114872311B (zh) * 2021-02-05 2023-11-14 合肥元顿传感科技有限公司 自动覆膜装置

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