WO2017175400A1 - 表面被覆切削工具およびその製造方法 - Google Patents
表面被覆切削工具およびその製造方法 Download PDFInfo
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- WO2017175400A1 WO2017175400A1 PCT/JP2016/068500 JP2016068500W WO2017175400A1 WO 2017175400 A1 WO2017175400 A1 WO 2017175400A1 JP 2016068500 W JP2016068500 W JP 2016068500W WO 2017175400 A1 WO2017175400 A1 WO 2017175400A1
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- layer
- grain boundaries
- crystal
- hard layer
- crystal grains
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- B23C2228/10—Coating
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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
- 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
Definitions
- the present invention relates to a surface-coated cutting tool and a manufacturing method thereof.
- This application claims priority based on Japanese Patent Application No. 2016-078297 filed on Apr. 8, 2016, and incorporates all the content described in the above Japanese application.
- Cutting tools made of cemented carbide often have problems that the cutting edge is worn or chipped because the cutting edge is exposed to a severe environment such as high temperature and high load during cutting. For this reason, development of the coating which coat
- a film made of a compound of titanium (Ti) and aluminum (Al) and / or nitrogen (N) and / or carbon (C) (hereinafter also referred to as AlTiN, AlTiCN, etc.) has high hardness. It is known that oxidation resistance can be improved by increasing the Al content. Improvement of the performance of the cutting tool is expected by coating the cutting tool with such a coating.
- Non-Patent Document 1 when Ikeda et al. (Non-Patent Document 1) produced a film of “AlTiN” or “AlTiCN” with an atomic ratio of Al exceeding 0.7 by a physical vapor deposition (PVD) method, It points out that the hardness decreases due to the phase transition of the structure to the wurtzite crystal structure.
- Setoyama et al. (Non-Patent Document 2) produced a TiN / AlN super-multilayer film by the PVD method in order to increase the Al content in the coating of “AlTiN” or “AlTiCN”.
- Patent Document 1 Japanese Patent Laying-Open No. 2015-193071
- Patent Document 1 is a hard coating layer formed by a CVD method and is represented by (Ti 1-x Al x ) (C y N 1-y ).
- a composite nitride layer or a composite carbonitride layer is included, the layer includes crystal grains having a cubic structure, and the composition of Ti and Al periodically changes along the normal direction of the surface of the tool substrate.
- a hard coating layer is disclosed.
- a surface-coated cutting tool is a surface-coated cutting tool including a substrate and a coating formed on the substrate, the coating including a hard layer, and the hard layer is chlorinated. It includes a plurality of crystal grains having a sodium-type crystal structure.
- the grain boundary of the crystal grain includes a CSL grain boundary and a general grain boundary, and the length of the ⁇ 3 type grain boundary among the CSL grain boundaries is the ⁇ 3 type grain boundary, ⁇ 7 type crystal grain constituting the CSL grain boundary.
- ⁇ 3-29 which is the total length of each of the boundary, ⁇ 11-type grain boundary, ⁇ 17-type crystal grain boundary, ⁇ 19-type crystal grain boundary, ⁇ 21-type crystal grain boundary, ⁇ 23-type crystal grain boundary, and ⁇ 29-type crystal grain boundary 50% or more of the type grain boundary length, and 1% or more and 30% or less of the total length of all grain boundaries, which is the sum of the length of the ⁇ 3-29 type grain boundary and the length of the general grain boundary. is there.
- the crystal grains include a first layer made of nitride or carbonitride of Al x Ti 1-x and a second layer made of nitride or carbonitride of Al y Ti 1-y (where x ⁇ y).
- the total thickness of the adjacent first and second layers is 3 nm or more and 30 nm or less.
- the manufacturing method of the surface coating cutting tool which concerns on 1 aspect of this invention is a manufacturing method of said surface coating cutting tool, Comprising: The 1st process which prepares a base material, A chemical vapor deposition (CVD) method is used for a hard layer.
- the second step includes the step of modulating the flow rate of either or both of the AlCl 3 gas and the TiCl 4 gas.
- Patent Document 1 the composite nitride layer or the composite carbonitride layer has a cubic structure, and the composition of Ti and Al periodically changes along the normal direction of the substrate, thereby achieving high hardness and toughness. It is said that an excellent hard coating layer was realized. However, this hard coating layer has room for improvement, particularly in obtaining chipping resistance. Therefore, it has not yet achieved the long life required by having both the high wear resistance and the high chipping resistance, and its development is eagerly desired.
- the present invention has been made in view of the above circumstances, and an object thereof is to provide a surface-coated cutting tool having high wear resistance and high chipping resistance, and a method for manufacturing the surface-coated cutting tool. [Effects of the present disclosure] According to the above, it is possible to provide a surface-coated cutting tool having high wear resistance and high chipping resistance.
- a surface-coated cutting tool is a surface-coated cutting tool including a base material and a coating formed on the base material, the coating including a hard layer, and the hard layer Includes a plurality of crystal grains having a sodium chloride type crystal structure, and the cross-section of the hard layer parallel to the normal direction of the surface of the substrate is subjected to electron beam backscatter diffraction apparatus to By analyzing the respective crystal orientations, the crossing angle between the normal direction with respect to the (001) plane which is the crystal plane of the crystal grain and the normal direction with respect to the surface of the substrate is measured.
- the crystal grain ratio A that is less than 50 degrees is 50% or more
- the grain boundary of the crystal grain includes a CSL grain boundary and a general grain boundary
- the length of the ⁇ 3 type grain boundary in the CSL grain boundary is ⁇ 3-type grain boundary, ⁇ 7-type crystal grain boundary, ⁇ 11-type crystal grain boundary, ⁇ 17-type crystal 50% or more of the length of the ⁇ 3-29 type grain boundary, which is the total length of the grain boundary, ⁇ 19 type grain boundary, ⁇ 21 type grain boundary, ⁇ 23 type grain boundary, and ⁇ 29 type grain boundary
- the total length of all grain boundaries which is the sum of the length of the ⁇ 3-29 type grain boundary and the length of the general grain boundary, is 1% or more and 30% or less
- the crystal grains are made of Al x Ti 1-x A laminated structure in which a first layer made of nitride or carbonitride and a second layer made of Al y Ti 1-y nitride or carbonitride (where x ⁇ y) are
- the above surface-coated cutting tool has high hardness and excellent toughness. Therefore, according to the surface-coated cutting tool, high wear resistance based on high hardness and high chipping resistance based on excellent toughness can be exhibited, and thus a long life can be realized.
- the hard layer has a crystal grain ratio B of 30% or more with an intersection angle of 10 degrees or more and less than 20 degrees. Thereby, the toughness of the surface-coated cutting tool is further improved.
- the hard layer has a thickness of 1 ⁇ m to 15 ⁇ m. Thereby, chipping resistance can be improved while maintaining the wear resistance of the surface-coated cutting tool.
- the hard layer has an indentation hardness of 28 GPa or more and 38 GPa or less by a nanoindentation method. This further improves the wear resistance of the surface-coated cutting tool.
- the hard layer has an absolute value of compressive residual stress of 0.5 GPa or more and 5.0 GPa or less. This further improves the toughness of the surface-coated cutting tool.
- a method for manufacturing a surface-coated cutting tool according to an aspect of the present invention is the above-described method for manufacturing a surface-coated cutting tool, wherein a first step of preparing a base material and a hard layer using a CVD method are prepared. A second step of forming, and the second step includes a step of modulating the flow rate of either or both of the AlCl 3 gas and the TiCl 4 gas.
- a surface-coated cutting tool capable of exhibiting high wear resistance based on high hardness and high chipping resistance based on excellent toughness and thus realizing a long life can be manufactured. can do.
- the notation in the form of “A to B” in the present specification means the upper and lower limits of the range (that is, not less than A and not more than B), and no unit is described in A, and only a unit is described in B. In this case, the unit of A and the unit of B are the same.
- a compound or the like when a compound or the like is represented by a chemical formula, when the atomic ratio is not particularly limited, it includes any conventionally known atomic ratio, and is not necessarily limited to a stoichiometric range.
- the surface-coated cutting tool includes a base material and a film formed on the base material.
- the coating preferably covers the entire surface of the substrate. However, even if a part of the substrate is not coated with this coating or the configuration of the coating is partially different, it does not depart from the scope of the present invention.
- FIG. 1 is a photograph of a microscopic image of a cross-section of a film in a surface-coated cutting tool.
- a coating 20 is provided on a substrate 10, and the coating 20 is composed of a hard layer.
- the surface-coated cutting tool according to this embodiment has high hardness and excellent toughness. For this reason, it is possible to exhibit high wear resistance based on high hardness and high chipping resistance based on excellent toughness, thereby realizing a long life. Therefore, drills, end mills, drill tip replacement cutting tips, end mill tip replacement cutting tips, milling tip replacement cutting tips, turning tip replacement cutting tips, metal saws, gear cutting tools, reamers, taps, etc. It can be suitably used as a cutting tool.
- any substrate can be used as long as it is conventionally known as this type of substrate.
- cemented carbide for example, WC-based cemented carbide, including WC, including Co or containing carbonitride such as Ti, Ta, Nb), cermet (TiC, TiN, TiCN, etc.) Main component
- high-speed steel ceramics (titanium carbide, silicon carbide, silicon nitride, aluminum nitride, aluminum oxide, etc.), cubic boron nitride sintered body, or diamond sintered body Is preferred.
- a cemented carbide particularly a WC-based cemented carbide, or a cermet (particularly a TiCN-based cermet).
- These base materials are particularly excellent in the balance between hardness and strength at high temperatures, and have excellent characteristics as base materials for surface-coated cutting tools for the above applications.
- the base material includes those having a chip breaker and those having no chip breaker.
- the shape of the edge of the cutting edge is sharp edge (the ridge where the rake face and flank face intersect), honing (the sharp edge is given a radius), negative land (the chamfered), honing and negative land combined. Any thing is included.
- the coating includes a hard layer.
- This hard layer may be included in the coating in one layer or two or more layers. It goes without saying that layers other than the hard layer may be included.
- the thickness of the coating is preferably 1 to 15 ⁇ m. When the thickness of the film is within this range, the characteristics of the film including the effect of improving the chipping resistance while maintaining the wear resistance of the hard layer can be suitably exhibited. If the thickness of the coating is less than 1 ⁇ m, the toughness tends to decrease, and if it exceeds 15 ⁇ m, the coating is easily peeled off from the substrate during cutting.
- the total thickness of the coating is preferably 3 to 7.5 ⁇ m from the viewpoint of improving the characteristics.
- the thickness of the coating is measured, for example, by obtaining a cross-sectional sample parallel to the normal direction of the surface of the substrate and observing the sample with a scanning transmission electron microscope (STEM).
- STEM high angle scattering dark field method HAADF-STEM: High-Angle Angular Dark-field Scanning Transmission Electron Microscopy
- the term “thickness” means an average thickness. Specifically, the observation magnification of the cross-sectional sample is set to 5000 to 10,000 times, the observation area is set to 100 to 500 ⁇ m 2 , the thickness width at 10 locations in one visual field is measured, and the average value is defined as “thickness”. The same applies to the thickness of each layer described later unless otherwise specified.
- the hard layer includes a plurality of crystal grains having a sodium chloride type crystal structure. It can be confirmed that the crystal grains contained in the hard layer have a sodium chloride type crystal structure using an X-ray diffractometer, a SEM-EBSD device, a TEM analyzer, or the like.
- the hard layer among the plurality of crystal grains confirmed in the observation region (100 ⁇ m ⁇ 100 ⁇ m) of the analyzer, 50 area% or more of crystal grains may have a sodium chloride type crystal structure. preferable. From the viewpoint of increasing the hardness of the hard layer, it is preferable that all the crystal grains contained in the hard layer are of a sodium chloride type.
- the crystal orientation of multiple crystal grains is analyzed using an electron back scatter diffraction (EBSD) device for the surface of the hard layer parallel to the normal direction of the substrate surface.
- EBSD electron back scatter diffraction
- the above-mentioned ratio A can be specifically obtained as follows. First, a hard layer is formed on a substrate based on a manufacturing method described later. It cut
- water-resistant abrasive paper containing a SiC abrasive abrasive as an abrasive
- the coating surface For example, after cutting the surface of the hard layer (if the other layer is formed on the hard layer, the coating surface) with a wax or the like on a sufficiently large holding plate. Then, cut with a rotary blade cutter in a direction perpendicular to the flat plate (cut so that the rotary blade and the flat plate are as vertical as possible). This is because the surface of the substrate and the surface of the hard layer (coating surface) are considered to be parallel. This cutting can be performed at any part of the hard layer as long as it is performed in such a vertical direction.
- the polishing is performed using the water-resistant abrasive papers # 400, # 800, and # 1500 in order (the number (#) of the water-resistant abrasive paper means a difference in the particle size of the abrasive, and the larger the number, the more abrasive particles. The diameter becomes smaller).
- the cross-section polished surface of the hard layer can be prepared. Then, this cross-section polished surface is used as a measurement target surface, and observation is performed using a field emission scanning electron microscope (FE-SEM) equipped with an EBSD device. This observation can be done by placing a focused electron beam individually on each pixel and collecting EBSD data in turn.
- the observation position is not particularly limited, but it is preferable to observe the vicinity of the edge of the edge of the blade in consideration of the relationship with the cutting characteristics.
- the EBSD device is based on automatic analysis of the Kikuchi diffraction pattern generated by backscattered electrons, and the crystal orientation in which crystal grains are oriented, and the crystal orientation is the normal direction of the measurement target surface (that is, the normal direction of the surface of the substrate) It is possible to measure the angle (intersection angle) at which the crossing is made. Using this, the measurement target plane is photographed using the above-described apparatus, and the intersection angle between the normal direction with respect to the (001) plane and the normal direction with respect to the surface of the substrate in each pixel of the photographed image is measured.
- the normal of the measurement target surface is inclined by 70 ° with respect to the incident beam, and analysis is performed at 15 kV. In order to avoid the charging effect, a pressure of 10 Pa is applied.
- the high current mode is used in combination with the opening diameter of 60 ⁇ m or 120 ⁇ m.
- Data collection is performed in steps of 0.1 ⁇ m / step for 500 ⁇ 300 pixels corresponding to a surface area of 50 ⁇ 30 ⁇ m in the measurement target surface. Then, the pixels are divided into the following intersection angle ranges, and groups 1 to 18 are constructed.
- Crossing angle is 0 degree or more and less than 5 degree
- Group 2 Crossing angle is 5 degree or more and less than 10 degree
- Group 3 Crossing angle is 10 degree or more and less than 15 degree
- Group 4 Crossing angle is 15 degree or more and less than 20 degree
- Group 5 Crossing angle between 20 and 25 degrees
- Group 6 Crossing angle between 25 and 30 degrees
- Group 7 Crossing angle between 30 and 35 degrees
- Group 8 Crossing angle between 35 and 40 degrees
- Group 9 Crossing Angle 10 to 45 degrees
- Group 10 Crossing angle 45 to 50 degrees
- Group 11 Crossing angle 50 to 55 degrees
- Group 12 Crossing angle 55 to 60 degrees
- Group 13 Crossing angle 60 degrees or more and less than 65 degrees
- Group 14 Crossing angle 65 degrees or more and less than 70 degrees
- Group 16 Crossing angle 75 degrees or more and less than 80 degrees
- Group 18 Crossing angle is 85 degrees or more and less than 90
- the frequency which is the sum of the number of pixels in each of the groups 1 to 18 is calculated, and the frequency distribution of the intersection angles is calculated. That is, “frequency” corresponds to the sum of the crystal grain areas of each group when all crystal grains appearing on the measurement target surface are divided into groups 1 to 18 for each crossing angle.
- the grouping and the calculation of the intersection angle frequency distribution can be performed using, for example, commercially available software ("Orientation Imaging Microscopy Ver 6.2", manufactured by EDAX).
- the vicinity of the interface on the substrate side of the hard layer and the vicinity of the interface on the surface side are excluded from the measurement target surface.
- the vicinity of the interface on the base material side of the hard layer is a portion formed at the initial stage of growth of the hard layer, and there is a large variation in crystal grains, which is inappropriate as a position where the characteristics of the hard layer should be specified.
- the observation magnification of the FE-SEM is appropriately selected from the range of 2000 to 20000 times, and the observation area is also appropriately selected from the range of 50 to 1000 ⁇ m 2 , and one field of view. It is preferable that 10 to 100 crystal grains appear.
- the ratio A is 50% or more when the total frequency of the groups 1 to 4 is 50% or more of the total frequency of all the groups. It will be. Since such a hard layer can have a high Young's modulus, the toughness of the coating can be improved.
- the ratio A is preferably 55% or more, and more preferably 60% or more.
- the ratio B of crystal grains in which the normal direction to the (001) plane is 10 degrees or more and less than 20 degrees with respect to the normal direction of the surface of the substrate is 30% or more.
- the total frequency of group 3 and group 4 is 30% or more of the total frequency of all groups.
- toughness can be dramatically improved.
- the ratio B is preferably 35% or more, and more preferably 40% or more. Note that the upper limit of the ratio B is 100%.
- the ratio B of the crystal grains having the crossing angle of 10 degrees or more and less than 20 degrees is another ratio. Is larger than that.
- the total frequency of group 3 and group 4 (corresponding to the ratio B) is the total frequency of group 1 and group 2, the total frequency of group 5 and group 6, and the frequency of group 7 and group 8.
- Total, frequency of group 9 and group 10, frequency of group 11 and group 12, frequency of group 13 and group 14, frequency of group 15 and group 16, and frequency of group 17 and group 18 It is preferable that it is larger than the sum total. In this case, the present inventors have confirmed that the defect resistance is particularly excellent.
- FIG. 2 An example of a graph showing the frequency distribution of crossing angles is shown in FIG.
- the horizontal axis of this graph represents 18 groups into which the crystal grains are divided, and the vertical axis is the frequency.
- the ratio A is 55% of the total frequency of all groups, and the ratio B is 39% of the total frequency of all groups.
- the grain boundaries of the crystal grains included in the hard layer include CSL grain boundaries (corresponding lattice crystal grain boundaries) and general grain boundaries, and the length of the ⁇ 3-type grain boundary among the CSL grain boundaries is CSL grain boundaries.
- the total grain boundary which is 50% or more of the length of the ⁇ 3-29 type grain boundary, which is the total length of each grain boundary, and is the sum of the length of the ⁇ 3-29 type grain boundary and the length of the general grain boundary
- the total length is 1% or more and 30% or less.
- the CSL grain boundary is characterized by a multiplicity index ⁇ , and corresponds to the case where the crystal lattice site densities of two crystal grains in contact with the crystal grain boundary are superimposed on both crystal lattices. It is defined as the ratio with the density of the part. For simple structures, it is generally accepted that low ⁇ value grain boundaries tend to have low interfacial energy and special properties. Therefore, the control of the ratio of the special grain boundaries and the distribution of grain orientation difference estimated from the CSL model is considered to be important for the characteristics of the ceramic coating and the method for improving these characteristics.
- CSL grain boundaries are ⁇ 3-type grain boundaries, ⁇ 7-type grain boundaries, ⁇ 11-type grain boundaries, ⁇ 17-type grain boundaries, ⁇ 19-type grain boundaries, ⁇ 21-type grain boundaries, and ⁇ 23-type crystal grains. And a ⁇ 29 type grain boundary.
- the general grain boundary is a grain boundary other than the CSL grain boundary. Therefore, the general grain boundary is a remaining portion obtained by removing the CSL grain boundary from the whole grain boundary of the crystal grains when the cross section of the hard layer is observed by EBSD.
- the length of the ⁇ 3 type grain boundary is the total length of the ⁇ 3 type grain boundary in the field of view observed by EBSD, as in the method for calculating the ratio A described above.
- the length is the ⁇ 3 type grain boundary, ⁇ 7 type grain boundary, ⁇ 11 type grain boundary, ⁇ 17 type grain boundary, ⁇ 19 type grain boundary, ⁇ 21 type grain boundary, ⁇ 23 type in the field of view observed by EBSD
- the total of the total length of each of the grain boundary and the ⁇ 29 type grain boundary is shown.
- the ⁇ 3-type grain boundary is considered to have the lowest grain boundary energy among the CSL grain boundaries. Therefore, by increasing the proportion of the ⁇ 3-29 type grain boundary in the ⁇ 3-29 type grain boundary, mechanical properties (particularly plastic resistance) It is thought that (deformability) can be improved.
- the ⁇ 3 type grain boundary is a grain boundary having high consistency, the two crystal grains having the ⁇ 3 type grain boundary as the grain boundary exhibit a behavior similar to that of a single crystal or twin crystal, and are coarsened. Show a tendency to When the crystal grains are coarsened, film properties such as chipping resistance deteriorate.
- the length of the ⁇ 3-type grain boundary is defined as 50% or more of the length of the ⁇ 3-29-type grain boundary, and the ⁇ 3-29 type It is defined as 1% or more and 30% or less of the total length of all grain boundaries, which is the sum of the lengths of crystal grain boundaries and general grain boundaries, thereby ensuring chipping resistance of the hard layer.
- the length of the ⁇ 3-type grain boundary is less than 90% of the length of the ⁇ 3-29 type grain boundary, and is the sum of the length of the ⁇ 3-29 type grain boundary and the length of the general grain boundary. It is preferably 1% or more and 15% or less of the total length of the grain boundaries. This is because a hard coating with uniform grain size and less variation in characteristics can be obtained.
- the length of the ⁇ 3-type grain boundary is 50% or more of the length of the ⁇ 3-29 type grain boundary can be confirmed as follows. First, a measurement sample having a measurement target surface is prepared by the same method as described in detail in (Orientation of crystal grains). Then, the surface to be measured is observed using an FE-SEM equipped with an EBSD device. Note that excluding the vicinity of the two interfaces of the hard layer from the measurement target surface is the same as described above.
- the normal of the measurement target surface is tilted by 70 ° with respect to the incident beam, and analysis is performed at 15 kV. In order to avoid the charging effect, a pressure of 10 Pa is applied.
- the high current mode is used in combination with the opening diameter of 60 ⁇ m or 120 ⁇ m.
- Data collection is performed at a step of 0.1 ⁇ m / step for 500 ⁇ 300 points corresponding to a surface area of 50 ⁇ 30 ⁇ m on the polished surface.
- the crystal grains contained in the hard layer are composed of a first layer made of nitride or carbonitride of Al x Ti 1-x and a nitride or carbonitride of Al y Ti 1-y (where x ⁇ y).
- the second layer is a laminated structure in which one or more layers are alternately laminated.
- the composition of the first layer and the second layer may be either nitride or carbonitride. However, when the composition of the first layer is nitride, the composition of the second layer is also nitride. When the composition of the first layer is carbonitride, the composition of the second layer is also carbonitride.
- the grains contained in the hard layer are AlTi nitride or carbonitride single crystals or twins, respectively, and the atomic ratio of Al varies within the single crystals or twins. ing. This variation is periodic and can be continuous or stepwise.
- the crystal grains included in the hard layer have a minute strain at a predetermined interface, and a laminated structure including a first layer and a second layer that can be distinguished as different layers based on the strain is formed. It becomes. And the hardness of a crystal grain improves with this distortion.
- FIG. 3 is an enlarged photograph showing the portion surrounded by the chain line in FIG.
- a white (light color) region is a region where the atomic ratio of Ti is larger than that of a black (dark color) region. That is, it can be understood from FIG. 3 that Ti-rich white areas and Al-rich black areas exist alternately in the hard layer.
- the ⁇ 3 type grain boundary exists as a line symmetry axis in the crystal structure in the twin crystal, and the above-described stacked structure exists on both sides of this axis. More preferred.
- the laminated structure can be stably grown over a long period.
- the atomic ratio x of Al in the first layer varies within the range of 0.76 or more and less than 1 in each first layer
- the atomic ratio y of Al in the second layer is 0. 0 in each second layer. It preferably varies within a range of 45 or more and less than 0.76. That is, the crystal grains contained in the hard layer fluctuate with the first layer in which the atomic ratio of Al is maintained to be high and the Al atomic ratio is relatively low in comparison with the first layer. It is preferable that the 2nd layer to have has the laminated structure arrange
- the atomic ratio x of Al in the first layer is never less than 0.76. This is because if the atomic ratio x is less than 0.76, it should be the Al atomic ratio y of the second layer. It is based on the same reason that atomic ratio y does not become 0.76 or more. The atomic ratio x does not become 1 because the first layer contains Ti. On the other hand, from the viewpoint of improving toughness while maintaining high wear resistance, the atomic ratio y is 0.45 or more. When the atomic ratio y is less than 0.45, the oxidation resistance becomes inferior due to the decrease in the amount of Al, and the toughness associated with the oxidation of the film tends to occur.
- the atomic ratio x and the atomic ratio y are obtained by obtaining a cross-sectional sample parallel to the normal direction of the surface of the substrate in the hard layer, and energy dispersive X-rays attached to the SEM or TEM with respect to the crystal grains appearing in the cross-sectional sample.
- EDX Energy Dispersive X-ray spectroscopy
- the atomic ratio at the analysis position can be calculated.
- the object for calculating the atomic ratio x and the atomic ratio y can be expanded to the entire surface of the cross-sectional sample, and therefore the atomic ratio x and The atomic ratio y can be specified.
- the maximum difference between the atomic ratio x and the atomic ratio y is 0.05 or more and 0.5 or less. Further, the maximum value of the difference between the atomic ratio x and the atomic ratio y is preferably 0.26 or more and 0.45 or less.
- the maximum value of the difference between the atomic ratio x and the atomic ratio y is less than 0.05, the strain in the crystal grains becomes small, and the hardness of the crystal grains tends to decrease.
- the maximum value of the difference exceeds 0.5, the strain in the crystal grains is too large and the lattice defects become large, so that the hardness of the crystal grains tends to decrease.
- the maximum value of the difference between the atomic ratio x and the atomic ratio y is calculated from the values of all the calculated atomic ratios x when the atomic ratio x and the atomic ratio y are calculated based on the cross-sectional sample by the above-described method. And the value obtained when the difference between the calculated maximum value of all the atomic ratios y and the minimum value is obtained. That is, it is synonymous with the value obtained when the difference between the maximum value of the atomic ratio x selected from the entire hard layer and the minimum value of the atomic ratio y is obtained.
- the total thickness (hereinafter also referred to as “stacking period”) of the adjacent first layer and second layer is 3 to 30 nm.
- the crystal grains have high hardness and toughness is improved.
- the total thickness of the adjacent first and second layers is preferably 5 to 25 nm.
- At least one pair of the adjacent first layer and second layer has a thickness of 3 to 30 nm.
- the total thickness of the adjacent first layer and second layer is, for example, obtained by obtaining a cross-sectional sample at an arbitrary location (preferably in the vicinity of the edge of the cutting edge), and 10 sets of 10 crystal grains appearing in the cross section.
- the total thickness of the first layer and the second layer adjacent to each other can be measured, and the average value can be expressed as the total thickness.
- the observation magnification is set to 500,000 and the observation area is set to about 0.1 ⁇ m 2 so that one crystal grain appears in one visual field.
- the crystal grains contained in the hard layer preferably have an average aspect ratio A of 2 or more.
- the maximum width among the widths of the individual crystal grains that are perpendicular to the crystal growth direction is defined as the particle width w, and the maximum of the lengths that are perpendicular to the grain width w.
- the grain length is 1 and the ratio of l to w (l / w) is the aspect ratio ⁇ of each crystal grain.
- an average value of the aspect ratio ⁇ obtained for each crystal grain is an average aspect ratio A
- an average value of the particle width w obtained for each crystal grain is an average grain width W.
- the crystal grains contained in the hard layer have an average aspect ratio A of 2 or more and an average particle width W of 0.5 ⁇ m or less.
- the crystal grains satisfying the above conditions have a columnar structure, which can exhibit excellent chipping resistance and wear resistance. If the average aspect ratio A of the crystal grains exceeds 100, it is not preferable because cracks easily propagate along the interface between the first layer and the second layer and the crystal grain boundary between the crystal grains.
- the average aspect ratio A of the crystal grains is preferably 30 to 80, more preferably 40 to 60. If the average grain width W of the crystal grains is less than 0.1 ⁇ m, the toughness decreases, which is not preferable. When the average grain width W of the crystal grains exceeds 1.0 ⁇ m, the wear resistance decreases. Therefore, the average grain width W of the crystal grains contained in the hard layer is preferably 0.1 to 1.0 ⁇ m.
- the average grain width W of the crystal grains is more preferably 0.2 to 0.8 ⁇ m.
- the average aspect ratio A can be measured, for example, by observing the surface to be measured with a STEM in the same manner as when measuring the thickness of the first layer and the second layer in the crystal grains. For example, ten crystal grains appearing in a STEM microscopic image are selected, and the particle width w and the particle length l are specified for these crystal grains. Next, the ratio (l / w) is calculated as the aspect ratio ⁇ of each crystal grain, and the average value of the aspect ratio ⁇ is calculated. Note that excluding the vicinity of the two interfaces of the hard layer from the measurement target surface is the same as described above.
- the hard layer preferably has an indentation hardness of 28 to 38 GPa by a nanoindentation method. More preferably, it is 30 to 36 GPa.
- the indentation hardness of the hard layer by the nanoindentation method is in the above range, the surface-coated cutting tool according to this embodiment has improved wear resistance. In particular, excellent performance can be achieved when cutting difficult-to-cut materials such as heat-resistant alloys.
- the above indentation hardness can be measured by using an ultra-fine indentation hardness tester that can use the nanoindentation method. Specifically, the indentation hardness can be calculated based on the indentation depth in which the indenter is pushed in with a predetermined load (for example, 30 mN) perpendicular to the thickness direction of the hard layer. When another layer such as a surface coating layer is present on the hard layer, the hard layer is exposed by excluding the surface coating layer by carrying out a calotest, oblique wrapping, etc., and the above method is applied to the exposed hard layer. By using it, indentation hardness can be measured.
- a predetermined load for example, 30 mN
- the hard layer preferably has a compressive residual stress, and the residual stress is preferably 0.5 GPa or more and 5 GPa or less. That is, when the hard layer has compressive residual stress, the absolute value is preferably 5 GPa or less. When the absolute value of the compressive residual stress of the hard layer is in the above range, the toughness of the hard layer can be dramatically improved. On the other hand, if the absolute value of the compressive residual stress exceeds 5 GPa, chipping tends to occur. When the hard layer has compressive residual stress, the absolute value is preferably 0.5 GPa or more. When the absolute value of compressive residual stress is less than 0.5 GPa, the toughness tends to decrease.
- the compressive residual stress of the hard layer can be controlled by adjusting the lamination period of the first layer and the second layer in the crystal grains included in the hard layer.
- compressive residual stress is a kind of internal stress (intrinsic strain) existing in the layer.
- the compressive residual stress is a stress represented by a numerical value “ ⁇ ” (minus) (in this specification, the unit is represented by “GPa”).
- ⁇ the degree of internal stress
- GPa the unit is represented by “GPa”.
- the compressive residual stress of the hard layer can be measured by, for example, the sin 2 ⁇ method using an X-ray stress measurement apparatus.
- the sin 2 ⁇ method using X-rays is widely used as a method for measuring the compressive residual stress of a polycrystalline material.
- “X-ray stress measurement method” Japan Society for Materials Science, published by Yokendo Co., Ltd. in 1981).
- Pages 54-67 can be used.
- When measuring the compressive residual stress of a hard layer by applying the sin 2 ⁇ method if there is another layer such as a surface coating layer on the hard layer, perform electrolytic polishing, flat milling, etc. as necessary. The hard layer is exposed except for the surface coating layer, and the compressive residual stress is measured for the exposed hard layer.
- the hard layer preferably has a thickness of 1 to 15 ⁇ m. When the thickness of the hard layer is within the above range, the effect of improving the chipping resistance while maintaining the wear resistance can be remarkably shown. If the thickness of the hard layer is less than 1 ⁇ m, the toughness is not sufficient, and if it exceeds 15 ⁇ m, chipping tends to occur.
- the thickness of the hard layer is more preferably 3 to 7.5 ⁇ m from the viewpoint of improving the characteristics.
- the hard layer does not affect the function and effect of this embodiment, chlorine (Cl), oxygen (O), boron (B), cobalt (Co), tungsten (W), chromium (Cr), tantalum (Ta) ), Niobium (Nb), carbon (C), and the like. That is, the hard layer is allowed to be formed including impurities such as inevitable impurities.
- the coating film may include a layer other than the hard layer.
- the base layer which can make the joining strength of a base material and a film high can be included.
- examples of such a layer include a TiN layer, a TiCN layer, a composite layer composed of a TiN layer and a TiCN layer, and the like.
- the underlayer can be produced by using a conventionally known production method.
- a compound layer composed of at least one element selected from the group consisting of Ti, Zr, and Hf and at least one element selected from the group consisting of N, O, C, B May be included.
- This compound layer can also increase the bonding strength between the substrate and the coating.
- the surface coating layer located on the outermost surface of the coating may include at least one of an ⁇ -Al 2 O 3 layer and a ⁇ -Al 2 O 3 layer. With the ⁇ -Al 2 O 3 layer and the ⁇ -Al 2 O 3 layer, the oxidation resistance of the coating can be improved.
- the surface-coated cutting tool according to this embodiment is used for, for example, high-speed intermittent cutting of stainless steel, occurrence of chipping, chipping, peeling, and the like can be suppressed. Because of its high hardness, it also exhibits wear resistance. Therefore, the surface-coated cutting tool according to the present embodiment can exhibit high wear resistance based on high hardness and high chipping resistance based on excellent toughness, thereby realizing a long life. .
- the manufacturing method of the surface coating cutting tool which concerns on this embodiment includes the 1st process of preparing a base material, and the 2nd process of forming a hard layer using CVD method.
- the second step includes a step of modulating the flow rate of AlCl 3 gas and / or TiCl 4 gas. Thereby, the surface coating cutting tool which has said structure and effect can be manufactured.
- the CVD apparatus 100 includes a plurality of base material holding jigs 21 for installing the base material 10 and a reaction vessel 22 made of heat resistant alloy steel surrounding the base material holding jig 21. ing.
- a temperature control device 23 for controlling the temperature in the reaction vessel 22 is provided around the reaction vessel 22.
- the gas introduced into the first gas introduction pipe 24 and the gas introduced into the second gas introduction pipe 25 are not mixed.
- a part of the first gas introduction pipe 24 and the second gas introduction pipe 25 is a base installed in the base material holding jig 21 with a gas flowing inside the first gas introduction pipe 24 and the second gas introduction pipe 25, respectively.
- a plurality of through holes for jetting on the material 10 are provided.
- reaction vessel 22 is provided with a gas exhaust pipe 27 for exhausting the gas inside the reaction vessel 22 to the outside.
- the gas inside the reaction vessel 22 passes through the gas exhaust pipe 27 and is discharged from the gas exhaust port 28 to the outside of the reaction vessel 22.
- a method for manufacturing a surface-coated cutting tool using the CVD apparatus 100 will be described.
- a case where a hard layer made of Al, Ti, and N is directly formed on a base material will be described.
- another layer such as a base layer is formed on the base material.
- the hard layer may be formed.
- a surface coating layer can also be formed in order to improve oxidation resistance. Conventionally known methods can be used for forming the underlayer and the surface coating layer.
- a substrate is prepared.
- a commercially available substrate may be used as the substrate, or it may be produced by a general powder metallurgy method.
- a mixed powder can be obtained by mixing WC powder and Co powder with a ball mill or the like. The mixed powder is dried and then molded into a predetermined shape to obtain a molded body. Further, the WC—Co cemented carbide (sintered body) is obtained by sintering the compact.
- a base material made of a WC—Co based cemented carbide can be manufactured by subjecting the sintered body to a predetermined cutting edge processing such as a honing process.
- a predetermined cutting edge processing such as a honing process.
- any conventionally known substrate can be prepared as this type of substrate, even if it is a substrate other than those described above.
- ⁇ Second step> In the second step, a hard layer is formed on the base material by a CVD method using the CVD apparatus 100.
- a chip having an arbitrary shape as the substrate 10 is mounted on the substrate holding jig 21 in the reaction vessel 22 of the CVD apparatus 100. Subsequently, the temperature of the substrate 10 placed on the substrate holding jig 21 is raised to 700 to 750 ° C. using the temperature control device 23. Further, the pressure inside the reaction vessel 22 is set to 2.0 to 3.0 kPa.
- a first gas group containing TiCl 4 gas and AlCl 3 gas is introduced into the first gas introduction pipe 24 while rotating the gas first gas introduction pipe 24 and the second gas introduction pipe 25 around the shaft 26.
- the second gas group containing NH 3 gas is introduced into the second gas introduction pipe 25.
- the ejected first gas group and second gas group are uniformly mixed in the reaction vessel 22 by a rotating operation, and the mixed gas is directed onto the substrate 10. And the nucleus of the crystal grain containing Al, Ti, and N is produced
- crystal grains are grown while modulating the flow rate of either or both of AlCl 3 gas and TiCl 4 gas.
- a first crystal growth method for modulating the flow rate of TiCl 4 gas, the TiCl 4 gas in the total reaction gas There is a second crystal growth method in which the flow rate of AlCl 3 gas is modulated while maintaining the flow rate constant.
- the atomic ratio of Ti can be controlled by adjusting the flow rate of the TiCl 4 gas (that is, the atomic ratio of Al can also be controlled). Specifically, the flow rate of TiCl 4 gas is maintained at 3 to 3% by volume (high flow) while maintaining the flow rate of AlCl 3 gas constant at 3 to 6% by volume for 3 to 15 seconds.
- the first gas group is introduced into the first gas introduction pipe 24. Immediately thereafter, switches the flow rate level of the TiCl 4 gas, the flow rate of TiCl 4 gas 0.2-0.8 vol% (low flow: Low Flow) the first gas group in conditions that maintain 3-15 seconds as a 1
- the gas is introduced into the gas introduction pipe 24. Thereafter, the flow rate of TiCl 4 gas is further switched. By repeating this operation a plurality of times, a hard layer containing crystal grains having a stacked structure in which the first layer and the second layer are alternately stacked can be formed.
- the atomic ratio of Al can be controlled by adjusting the flow rate of the AlCl 3 gas (that is, the atomic ratio of Ti can also be controlled). Specifically, while maintaining the flow rate of TiCl 4 gas constant at 0.5 to 1.5% by volume, the flow rate of AlCl 3 gas is set to 6 to 10% by volume (High Flow) for 5 to 15 seconds.
- the first gas group is introduced into the first gas introduction pipe 24 under the condition to be maintained. Immediately after that, the flow rate of the AlCl 3 gas is immediately switched, and the flow rate of the AlCl 3 gas is maintained at 1 to 4 volume% (low flow rate: Low Flow) for 5 to 15 seconds. 24. Thereafter, the flow rate of the AlCl 3 gas is further switched. By repeating this operation a plurality of times, a hard layer containing crystal grains having a stacked structure in which the first layer and the second layer are alternately stacked can be formed.
- a high flow rate (High Flow) in TiCl 4 times for jetting gas or AlCl 3 gas, low flow (Low Flow) at the time of ejecting a TiCl 4 gas or AlCl 3 gas By adjusting the number of times of switching the flow rate of TiCl 4 gas or AlCl 3 gas from a high flow rate to a low flow rate or from a low flow rate to a high flow rate, the thicknesses of the first layer and the second layer, the adjacent first layer and The total thickness with the second layer and the thickness of the hard layer can each be controlled to a desired thickness.
- the orientation of crystal grains contained in the hard layer can be controlled so as to satisfy the above ratio A.
- the length of the ⁇ 3 type crystal grain boundary is set to 50% or more of the length of the ⁇ 3-29 type crystal grain boundary.
- the total length of all grain boundaries which is the sum of the length of the ⁇ 3-29 type grain boundary and the length of the general grain boundary, can be 1% or more and 30% or less.
- the first gas group preferably contains hydrogen chloride (HCl) gas and hydrogen (H 2 ) gas as a carrier gas, together with TiCl 4 and AlCl 3 gas.
- the second gas group preferably contains argon gas together with NH 3 gas.
- nitrogen (N 2 ) gas may be included.
- nitrogen (N 2 ) gas is not included, and only ammonia (NH 3 ) gas and argon gas are used.
- the second gas group is preferably configured.
- the hard layer can be formed, and the surface-coated cutting tool according to this embodiment can be manufactured.
- the surface to be measured used for each measurement was prepared by polishing a cross section parallel to the normal direction of the surface of the substrate with water-resistant abrasive paper as described above, and then further smoothing by an ion milling treatment with Ar ions.
- the ion milling apparatus and its processing conditions are as follows. Ion milling device: “SM-09010”, JEOL Ltd. acceleration voltage: 6 kV Irradiation angle: 0 ° from the normal direction of the substrate surface Irradiation time: 6 hours.
- the total thickness of the coating, the thickness of each layer such as the hard layer, the presence of the first layer and the second layer in the crystal grains, and the average value (lamination cycle) of the total thickness of the adjacent first layer and second layer are:
- the measurement was performed by observing the surface to be measured using the STEM high-angle scattering dark field method using STEM (“JEM-2100F”, manufactured by JEOL Ltd.).
- the crystal structure of the crystal grains contained in the hard layer was confirmed by an X-ray diffractometer (“SmartLab”, manufactured by Rigaku Corporation).
- the atomic ratio x of Al in the first layer and the atomic ratio y of Al in the second layer are calculated by an EDX apparatus (“SD100GV”, manufactured by JEOL Ltd.) attached to the TEM, and the calculated atomic ratios x and y The maximum value of xy was determined based on the value.
- SD100GV manufactured by JEOL Ltd.
- An FE ⁇ equipped with an EBSD device is used for the measurement of the frequency distribution of the crossing angles for calculating the ratio A and the ratio B, and the measurement of the length of the ⁇ 3 type grain boundary and the length of the ⁇ 3-29 type grain boundary.
- SEM Zero-Fi Supra 35 VP”, CARL ZEISS
- the indentation hardness (GPa) of the hard layer by the nanoindentation method was measured using an ultra-fine indentation hardness tester (“ENT-1100a”, manufactured by Elionix).
- the compressive residual stress (GPa) of the hard layer was calculated by the sin 2 ⁇ method using an X-ray stress measuring device (“SmartLab”, manufactured by Rigaku Corporation).
- SmartLab manufactured by Rigaku Corporation
- the physical property coefficient used for the stress measurement is N.K.
- the values reported in Norrby et al., “Surface & Coatings Technology 257 (2014) 102-107)” were used.
- it is preferable to measure the stress by selecting the diffraction peak on the high angle side so that the peaks of the first hard coating layer and the substrate do not overlap as much as possible in consideration of the type of the substrate used.
- a substrate A and a substrate B were prepared. Specifically, raw material powders having the composition (% by mass) shown in Table 1 were uniformly mixed. “Remaining” in Table 1 indicates that WC occupies the remainder of the composition (mass%).
- the mixed powder is pressed into a predetermined shape and then sintered at 1300 to 1500 ° C. for 1 to 2 hours, whereby a base material A (shape: CNMG120408NUX) and a base material B (made of cemented carbide) Shape: SEET13T3AGSN-G) was obtained.
- the base layer (TiN and TiN and TiCN depending on the sample) of the composition shown in Table 2 was formed on the surface of the base material A and the base material B with the thickness as shown in Table 9.
- a hard layer which will be described later, was formed on the underlayer with a thickness as shown in Table 9.
- a surface coating layer (Al 2 O 3 ) was also formed depending on the sample.
- the underlayer is a layer that is in direct contact with the surface of the substrate.
- a surface coating layer is a layer formed on a hard layer, and comprises the surface of a cutting tool.
- reaction gas composition volume%
- pressure kPa
- temperature ° C.
- reaction atmosphere a condition of the total gas flow rate
- TiN layer the substrate was placed in a reaction vessel of a known CVD apparatus comprising a CVD apparatus 100 shown in FIG. 4, 2.0 vol% of TiCl 4 gas into the reaction vessel, 39. It can be formed by injecting a mixed gas composed of 7% by volume of N 2 gas and the balance H 2 gas at a total gas flow rate of 44.7 L / min in an atmosphere having a pressure of 6.7 kPa and a temperature of 915 ° C. . The thickness of each layer can be controlled by the time during which the reaction gas is ejected.
- the hard layer was formed using a CVD apparatus 100 as shown in FIG. 4 under any one of the formation conditions 1A to 1H, 2A to 2H, X and Y shown in Tables 3 to 5.
- the first crystal growth method of growing crystal grains by modulating the flow rate of TiCl 4 gas while maintaining the flow rate of AlCl 3 gas constant was used.
- a second crystal growth method in which crystal grains are grown by modulating the flow rate of the AlCl 3 gas while keeping the flow rate of the TiCl 4 gas constant is used.
- crystal grains were grown by intermittently supplying the first gas group and the second gas group while keeping the flow rates of the AlCl 3 gas and the TiCl 4 gas constant without modulation. Specifically, the first gas group and the second gas group were supplied at a cycle of stopping for 0.8 seconds and ejecting for 0.2 seconds.
- the flow rate of the AlCl 3 gas and the TiCl 4 gas was kept constant, and the crystal grains were grown by performing continuous gas ejection.
- the formation condition “1A” indicates that the hard layer is formed under the following conditions. That is, the film forming temperature (base material temperature) is set to 750 ° C., the pressure in the reaction vessel is set to 3.0 kPa, and the total gas flow rate that is the sum of the flow rates of the first gas group and the second gas group is set to 60.5 L / min. To do. Under this condition, the first gas group is maintained under the condition that the flow rate of the AlCl 3 gas is kept constant at 5% by volume, and the TiCl 4 gas is maintained at 0.5% by volume (Low Flow) for 3 seconds (Time). Is introduced into the first gas introduction pipe 24.
- the TiCl 4 gas flow rate is switched between high and low, and the AlCl 3 gas flow rate is maintained at the above concentration, and the TiCl 4 gas flow rate is 1.5 vol% (high flow rate: High Flow) and maintained for 3 seconds (Time).
- the first gas group is introduced into the first gas introduction pipe 24 under the conditions to be satisfied. Thereafter, the flow rate of the TiCl 4 gas is further switched, and such an operation is performed a plurality of times as desired.
- the TiCl 4 gas is introduced into the first gas introduction pipe 24 at intervals of 3 seconds per minute at high and low flow rates 10 times (Interval).
- the first gas group includes TiCl 4 gas and AlCl 3 gas, and H 2 gas as the balance.
- the second gas group includes each predetermined amount (volume%) of NH 3 gas and Ar gas.
- the flow rate of TiCl 4 or AlCl 3 was modulated in the same manner as “1A”, and a hard layer was formed under the conditions shown in Table 3 or Table 4.
- the hard layer was formed under the conditions shown in Table 5.
- crystal grains having a laminated structure of the first layer and the second layer made of AlTi nitride grew.
- ethylene gas is contained in the first gas group in the volume% as shown in Tables 3 and 4, so that the carbonitride of AlTi
- the crystal grains having the laminated structure of the first layer and the second layer made of were grown.
- the hard layer formed under each of the above conditions is formed by growing crystal grains having a stacked structure in which the first layer and the second layer are alternately stacked at the stacking cycle as shown in Tables 6 to 8. .
- Tables 6 to 8 the thickness of the first layer, the thickness of the second layer, the atomic ratio x (maximum value) of Al in the first layer, and the atomic ratio y (minimum value) of Al in the second layer formed according to each condition. ), The difference between the atomic ratio x (maximum value) and the atomic ratio y (minimum value) (xy), the ratio of the length of the ⁇ 3-type grain boundary to the length of the ⁇ 3-29 type grain boundary (Table 6).
- ⁇ 3 length / ⁇ 3-29 length (%) the ratio of the total length of all grain boundaries, which is the sum of the length of the ⁇ 3-29 type grain boundary and the length of the general grain boundary.
- ⁇ 3 length / total length of all grain boundaries (%) the ratio A and the ratio B, which are the frequencies of the crossing angles of the crystal grains contained in the hard layer, are also shown.
- All of the crystal grains contained in the hard layer formed under the formation conditions 1A to 1H and 2A to 2H had a sodium chloride type crystal structure. All the crystal grains contained in the hard layer formed under the formation conditions X and Y also had a sodium chloride type crystal structure.
- ⁇ Making cutting tools The base material A or base material B prepared as described above was coated with a film by the method as described above, and sample Nos. As shown in Table 9 were used. 1 to 36 cutting tools were produced. In this example, sample No. The cutting tools 1 to 32 are examples. 33 to 36 cutting tools are comparative examples.
- any of the base material, the base layer, and the hard layer is different for each sample.
- Table 9 when two compounds (for example, “TiN (0.5) -TiCN (2.5)”) are listed in one column, the left side (“TiN (0.5)”) It means that the compound is a layer located on the side close to the surface of the substrate, and the right side (“TiCN (2.5)”) compound is a layer located on the side far from the surface of the substrate.
- the numbers in parentheses mean the thickness of each layer.
- the column indicated by “ ⁇ ” in Table 9 means that no layer is present.
- sample no The values of indentation hardness and compressive residual stress of the hard layer in the cutting tools 1 to 36 are also shown.
- the surface coating layer Al 2 O 3 layer
- Sample No. The thickness of the entire coating film of 1 cutting tool is 9.0 ⁇ m.
- Sample No. The indentation hardness (GPa) exhibited by the hard layer in the cutting tool 1 is 34.3, and the compressive residual stress (GPa) is 3.3.
- sample no. The cutting tools Nos. 9 to 16 and 25 to 32 are sample Nos. It was confirmed that it has a long life compared with the cutting tools of 35 and 36. In particular, sample no. Chipping of the cutting tool No. 35 was confirmed, and sample No. It was confirmed that the cutting tool 36 was inferior in chipping resistance (chip resistance).
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Abstract
Description
特許文献1では、複合窒化物層または複合炭窒化物層が立方晶構造を有し、TiおよびAlの組成が基体の法線方向に沿って周期的に変化することにより、高硬度かつ靱性にも優れる硬質被覆層を実現したとされている。しかしながら、この硬質被覆層は特に耐チッピング性の獲得において改善の余地があった。したがって、未だ高い耐摩耗性と高い耐チッピング性との両特性を有することによって要求される長寿命を実現することには至っておらず、その開発が切望されている。
[本開示の効果]
上記によれば、高い耐摩耗性と高い耐チッピング性とを有する表面被覆切削工具を提供することができる。
最初に本発明の実施態様を列記して説明する。
以下、実施形態について説明する。以下の実施形態の説明に用いられる図面において、同一の参照符号は、同一部分または相当部分を表わす。
本実施形態に係る表面被覆切削工具は、基材と、該基材上に形成された被膜とを備える。被膜は、基材の全面を被覆することが好ましい。しかしながら、基材の一部がこの被膜で被覆されていなかったり被膜の構成が部分的に異なっていたりしていたとしても、本発明の範囲を逸脱するものではない。
基材は、この種の基材として従来公知のものであればいずれも使用することができる。たとえば、超硬合金(たとえば、WC基超硬合金、WCのほか、Coを含み、あるいはTi、Ta、Nbなどの炭窒化物を添加したものも含む)、サーメット(TiC、TiN、TiCNなどを主成分とするもの)、高速度鋼、セラミックス(炭化チタン、炭化ケイ素、窒化ケイ素、窒化アルミニウム、酸化アルミニウムなど)、立方晶型窒化ホウ素焼結体、またはダイヤモンド焼結体のいずれかであることが好ましい。
本実施形態において被膜は、硬質層を含む。この硬質層は、当該被膜中に1層または2層以上含まれることができる。また硬質層以外の他の層を含んでもよいことはいうまでもない。
(結晶粒の結晶構造)
硬質層は、塩化ナトリウム型の結晶構造を有する複数の結晶粒を含む。硬質層に含まれる結晶粒が塩化ナトリウム型の結晶構造を有していることは、X線回折装置、SEM-EBSD装置、TEM分析装置などを用いて確認することができる。
硬質層において、硬質層のうち基材の表面の法線方向に平行な面に対し、電子線後方散乱回折(EBSD:Electron Back Scatter Diffraction)装置を用いて複数の結晶粒の結晶方位をそれぞれ解析することにより、結晶粒の結晶面である(001)面に対する法線方向と基材の表面に対する法線方向との交差角を測定した場合に、交差角が0度以上20度未満となる結晶粒の割合Aが50%以上である。硬質層がこれを満たす場合に、硬質層は靱性に特に優れることとなり、もって表面被覆切削工具の優れた耐チッピング性に寄与することができる。上記割合の上限値は特に限定されず、靱性の向上の観点からは100%が好ましい。
グループ2:交差角が5度以上10度未満
グループ3:交差角が10度以上15度未満
グループ4:交差角が15度以上20度未満
グループ5:交差角が20度以上25度未満
グループ6:交差角が25度以上30度未満
グループ7:交差角が30度以上35度未満
グループ8:交差角が35度以上40度未満
グループ9:交差角が40度以上45度未満
グループ10:交差角が45度以上50度未満
グループ11:交差角が50度以上55度未満
グループ12:交差角が55度以上60度未満
グループ13:交差角が60度以上65度未満
グループ14:交差角が65度以上70度未満
グループ15:交差角が70度以上75度未満
グループ16:交差角が75度以上80度未満
グループ17:交差角が80度以上85度未満
グループ18:交差角が85度以上90度未満。
硬質層に含まれる複数の結晶粒間には、結晶粒の粒界である「結晶粒界」が存在する。特に、硬質層に含まれる結晶粒の結晶粒界は、CSL粒界(対応格子結晶粒界)と一般粒界とを含み、CSL粒界のうちΣ3型結晶粒界の長さは、CSL粒界を構成するΣ3型結晶粒界、Σ7型結晶粒界、Σ11型結晶粒界、Σ17型結晶粒界、Σ19型結晶粒界、Σ21型結晶粒界、Σ23型結晶粒界、およびΣ29型結晶粒界のそれぞれの長さの総計であるΣ3-29型結晶粒界の長さの50%以上で、Σ3-29型結晶粒界の長さと一般粒界の長さとの和である全粒界の合計長さの1%以上30%以下である。
硬質層に含まれる結晶粒は、AlxTi1-xの窒化物または炭窒化物からなる第1層と、AlyTi1-yの窒化物または炭窒化物(ただし、x≠y)からなる第2層とが交互に1層以上積層された積層構造を有している。第1層および第2層の組成は、窒化物または炭窒化物のいずれでもよい。ただし、第1層の組成が窒化物となる場合、第2層の組成も窒化物となる。第1層の組成が炭窒化物となる場合、第2層の組成も炭窒化物となる。
本実施形態において、隣り合う第1層と第2層との厚みの合計(以下、「積層周期」とも称する)は、3~30nmである。このような厚みで第1層と第2層とからなる積層構造を有することにより、結晶粒は高硬度となり、かつ靱性が向上する。この厚みが30nmを超えると、結晶粒がウルツ鉱型結晶構造へ相転移することにより硬度が低下する傾向があり、耐摩耗性に悪影響が及ぶ。隣り合う第1層と第2層との厚みの合計は、好ましくは5~25nmである。
本実施形態において硬質層に含まれる結晶粒は、平均アスペクト比Aが2以上であることが好ましい。本実施形態では、個々の結晶粒において結晶の成長方向に垂直な方向となる幅のうち最大のものを粒子幅wとし、この粒子幅wに対して垂直な方向となる長さのうち最大のものを粒子長さlとし、wとlとの比(l/w)を個々の結晶粒のアスペクト比αとする。さらに、個々の結晶粒について求めたアスペクト比αの平均値を平均アスペクト比A、個々の結晶粒について求めた粒子幅wの平均値を平均粒子幅Wとする。このとき、硬質層に含まれる結晶粒は、平均アスペクト比Aが2以上であり、かつ平均粒子幅Wが0.5μm以下であることがより好ましい。
硬質層は、ナノインデンテーション法による押し込み硬さが28~38GPaであることが好ましい。より好ましくは、30~36GPaである。硬質層のナノインデンテーション法による押し込み硬さが上記範囲であることにより、本実施形態に係る表面被覆切削工具は、耐摩耗性が向上する。特に、耐熱合金などの難削材の切削加工を行う際に優れた性能を発揮することができる。
硬質層は、圧縮残留応力を有することが好ましく、該残留応力は、0.5GPa以上5GPa以下であることが好ましい。すなわち硬質層が圧縮残留応力を有する場合、その絶対値は5GPa以下であることが好ましい。硬質層の圧縮残留応力の絶対値が上記範囲であることにより、硬質層の靱性を飛躍的に向上させることができる。一方、圧縮残留応力の絶対値が5GPaを超えると、チッピングが起きやすくなる傾向がある。また硬質層が圧縮残留応力を有する場合、その絶対値は0.5GPa以上であることが好ましい。圧縮残留応力の絶対値が0.5GPa下回ると、靱性が低下する傾向がある。硬質層の圧縮残留応力は、硬質層に含まれる結晶粒内における第1層と第2層との積層周期を調節することによって制御することができる。
硬質層は、1~15μmの厚みを有することが好ましい。硬質層の厚みが上記範囲であることにより、耐摩耗性を維持しつつ耐チッピング性を向上させる効果を顕著に示すことができる。硬質層の厚みが1μm未満であると靱性が十分ではなく、15μmを超えるとチッピングが起きやすくなる傾向がある。硬質層の厚みは、その特性を向上させる観点から3~7.5μmであることがさらに好ましい。
硬質層は、本実施形態の作用効果に影響を及ぼさない限り、塩素(Cl)、酸素(O)、硼素(B)、コバルト(Co)、タングステン(W)、クロム(Cr)、タンタル(Ta)、ニオブ(Nb)、炭素(C)などを含んでいてもよい。すなわち硬質層は、不可避不純物などの不純物を含んで形成されることが許容される。
本実施形態において被膜は、硬質層以外の層を含んでいてもよい。たとえば、基材と被膜との接合強度を高くすることが可能な下地層を含むことができる。そのような層として、たとえば、TiN層、TiCN層、TiN層とTiCN層とからなる複合層などを挙げることができる。下地層は、従来公知の製造方法を使用することにより製造することができる。
本実施形態に係る表面被覆切削工具は、たとえば、ステンレス鋼の高速断続切削などに用いた場合であっても、チッピング、欠損、剥離などの発生が抑えられる。高硬度であるので耐摩耗性も発揮する。したがって、本実施形態に係る表面被覆切削工具は、高硬度に基づいた高い耐摩耗性と、優れた靱性に基づいた高い耐チッピング性能とを示すことができ、もって長寿命を実現することができる。
本実施形態に係る表面被覆切削工具の製造方法は、基材を準備する第1工程と、硬質層をCVD法を用いて形成する第2工程とを含む。特に、第2工程は、AlCl3ガスおよびTiCl4ガスの両方またはいずれか一方の流量を変調させる工程を含む。これにより、上記の構成および効果を有する表面被覆切削工具を製造することができる。
第1工程では基材を準備する。基材は、市販のものを用いてもよく、一般的な粉末冶金法で製造してもよい。たとえば、基材として超硬合金基材を一般的な粉末冶金法で製造する場合、ボールミルなどによってWC粉末とCo粉末などとを混合して混合粉末を得ることができる。該混合粉末を乾燥した後、所定の形状に成形して成形体を得る。さらに該成形体を焼結することにより、WC-Co系超硬合金(焼結体)を得る。次いで該焼結体に対して、ホーニング処理などの所定の刃先加工を施すことにより、WC-Co系超硬合金からなる基材を製造することができる。第1工程では、上記以外の基材であっても、この種の基材として従来公知のものをいずれも準備可能である。
第2工程では、CVD装置100を用いたCVD法により、基材上に硬質層を形成する。
各測定に用いた測定対象面は、基材の表面の法線方向に平行な断面を上述のとおり耐水研磨紙で研磨し、引続き、Arイオンによるイオンミーリング処理によりさらに平滑化して準備した。イオンミーリング装置とその処理の条件は以下のとおりである。
イオンミーリング装置:「SM-09010」、日本電子株式会社製
加速電圧: 6kV
照射角度: 基材表面の法線方向から0°
照射時間: 6時間。
第1工程として、基材Aおよび基材Bを準備した。具体的には、表1に記載の配合組成(質量%)からなる原料粉末を均一に混合した。なお表1中の「残り」とは、WCが配合組成(質量%)の残部を占めることを示す。次に、この混合粉末を所定の形状に加圧成形した後に、1300~1500℃で1~2時間焼結することにより、超硬合金からなる基材A(形状:CNMG120408NUX)および基材B(形状:SEET13T3AGSN-G)を得た。これらの形状は、いずれも住友電工ハードメタル株式会社製のものであり、基材AであるCNMG120408NUXは、旋削用の刃先交換型切削チップの形状であり、基材BであるSEET13T3AGSN-Gは、転削(フライス)用の刃先交換型切削チップの形状である。
第2工程として、基材Aおよび基材Bの表面上に表2に示す組成の下地層(TiN、試料によってはTiNおよびTiCN)を、表9に示すとおりの厚みで形成した。下地層上に後述する硬質層を表9に示すとおりの厚みで形成した。そのほか表9に示すとおり、試料によっては表面被覆層(Al2O3)も形成した。下地層は基材の表面と直接接する層である。表面被覆層は、硬質層上に形成される層であって切削工具の表面を構成する。
硬質層の形成は、図4に示すようなCVD装置100を用い、表3~表5に示す形成条件1A~1H、2A~2H、XおよびYのいずれかの条件で行なった。
上述のように準備された基材Aまたは基材Bを、上記のような方法で被膜により被覆し、表9に示すとおりの試料No.1~36の切削工具を作製した。本実施例において試料No.1~32の切削工具が実施例であり、試料No.33~36の切削工具が比較例である。
上記のようにして作製した試料No.1~36の切削工具を用いて、以下の2種の切削試験を行った。
試料No.1~8、17~24、33および34の切削工具について、以下の切削条件により逃げ面摩耗量(Vb)が0.20mmとなるまでの切削時間を測定するとともに刃先の最終損傷形態を観察し、工具寿命を評価した。その結果を表10に示す。切削時間が長いほど耐摩耗性に優れる切削工具として、高速切削であっても長寿命化を実現することができる可能性が高いと評価することができる。
被削材 : FCD450丸棒
周速 : 500m/min
送り速度: 0.15mm/rev
切込み量: 1.0mm
切削液 : 有り。
試料No.9~16、25~32、35および36の切削工具について、以下の切削条件により逃げ面摩耗量(Vb)が0.20mmとなるまでの切削距離を測定するとともに刃先の最終損傷形態を観察し、工具寿命を評価した。その結果を表11に示す。切削距離が長いほど耐チッピング性に優れる切削工具として、被削材の種類に関わらず長寿命化を実現することができる可能性が高いと評価することができる。
被削材 : SUS304ブロック材
周速 : 250m/min
送り速度: 0.3mm/s
切込み量: 2.0mm
切削液 : なし
カッタ : WGC4160R(住友電工ハードメタル株式会社製)。
表10によれば、試料No.1~8、17~24の切削工具は、試料No.33および34の切削工具と比べて長寿命であることが確認された。特に、試料No.33および34の切削工具は、チッピングが確認されて高速切削に対して性能が劣ることが確認された。
Claims (6)
- 基材と、該基材上に形成された被膜とを備える表面被覆切削工具であって、
前記被膜は、硬質層を含み、
前記硬質層は、塩化ナトリウム型の結晶構造を有する複数の結晶粒を含み、
前記硬質層のうち前記基材の表面の法線方向に平行な断面に対し、電子線後方散乱回折装置を用いて前記複数の結晶粒の結晶方位をそれぞれ解析することにより、前記結晶粒の結晶面である(001)面に対する法線方向と前記基材の表面に対する法線方向との交差角を測定した場合に、前記交差角が0度以上20度未満となる前記結晶粒の割合Aが50%以上であり、
前記結晶粒の粒界は、CSL粒界と、一般粒界とを含み、
前記CSL粒界のうちΣ3型結晶粒界の長さは、前記CSL粒界を構成するΣ3型結晶粒界、Σ7型結晶粒界、Σ11型結晶粒界、Σ17型結晶粒界、Σ19型結晶粒界、Σ21型結晶粒界、Σ23型結晶粒界、およびΣ29型結晶粒界のそれぞれの長さの総計であるΣ3-29型結晶粒界の長さの50%以上で、前記Σ3-29型結晶粒界の長さと前記一般粒界の長さとの和である全粒界の合計長さの1%以上30%以下であり、
前記結晶粒は、AlxTi1-xの窒化物または炭窒化物からなる第1層と、AlyTi1-yの窒化物または炭窒化物(ただしx≠y)からなる第2層とが交互に積層された積層構造を有し、
隣り合う前記第1層と前記第2層との厚みの合計は、3nm以上30nm以下である、表面被覆切削工具。 - 前記交差角が10度以上20度未満となる前記結晶粒の割合Bが、30%以上である、請求項1に記載の表面被覆切削工具。
- 前記硬質層は、1μm以上15μm以下の厚みを有する、請求項1または請求項2に記載の表面被覆切削工具。
- 前記硬質層は、ナノインデンテーション法による押し込み硬さが28GPa以上38GPa以下である、請求項1から請求項3のいずれか1項に記載の表面被覆切削工具。
- 前記硬質層は、圧縮残留応力の絶対値が0.5GPa以上5.0GPa以下である、請求項1から請求項4のいずれか1項に記載の表面被覆切削工具。
- 請求項1から請求項5のいずれか1項に記載の表面被覆切削工具の製造方法であって、
前記基材を準備する第1工程と、
前記硬質層を化学蒸着法を用いて形成する第2工程とを含み、
前記第2工程は、AlCl3ガスおよびTiCl4ガスの両方またはいずれか一方の流量を変調させながら前記結晶粒を成長させる工程を含む、表面被覆切削工具の製造方法。
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JP7124236B1 (ja) * | 2021-06-14 | 2022-08-23 | 住友電工ハードメタル株式会社 | 切削工具 |
WO2022264196A1 (ja) * | 2021-06-14 | 2022-12-22 | 住友電工ハードメタル株式会社 | 切削工具 |
WO2022264197A1 (ja) * | 2021-06-14 | 2022-12-22 | 住友電工ハードメタル株式会社 | 切削工具 |
WO2022264198A1 (ja) * | 2021-06-14 | 2022-12-22 | 住友電工ハードメタル株式会社 | 切削工具 |
US11534837B1 (en) | 2021-06-14 | 2022-12-27 | Sumitomo Electric Hardmetal Corp. | Cutting tool |
Also Published As
Publication number | Publication date |
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CN107438491A (zh) | 2017-12-05 |
US10166611B2 (en) | 2019-01-01 |
EP3415255A4 (en) | 2019-04-03 |
EP3415255B1 (en) | 2020-03-04 |
US20180178294A1 (en) | 2018-06-28 |
JP2017185610A (ja) | 2017-10-12 |
KR102312226B1 (ko) | 2021-10-14 |
JP6044861B1 (ja) | 2016-12-14 |
KR20180128822A (ko) | 2018-12-04 |
CN107438491B (zh) | 2020-02-07 |
EP3415255A1 (en) | 2018-12-19 |
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