JP4666211B2 - Surface-coated cermet cutting tool with excellent chipping resistance thanks to thick α-type aluminum oxide layer - Google Patents

Description

In the present invention, an upper layer of a hard coating layer, that is, an aluminum oxide layer (hereinafter referred to as an α-type Al ₂ O ₃ layer) having an α-type crystal structure in a state where chemical vapor deposition is formed is particularly thick. The present invention relates to a surface-coated cermet cutting tool (hereinafter referred to as a coated cermet tool) that exhibits excellent chipping resistance even when used for cutting various steels and cast iron.

Conventionally, generally on the surface of a substrate (hereinafter collectively referred to as a tool substrate) composed of a tungsten carbide (hereinafter referred to as WC) -based cemented carbide or titanium carbonitride (hereinafter referred to as TiCN) -based cermet. ,
(A) As a lower layer, a Ti carbide (hereinafter referred to as TiC) layer, nitride (hereinafter also referred to as TiN) layer, carbonitride (hereinafter referred to as TiCN) layer formed by chemical vapor deposition, Ti composed of one or more of a carbon oxide (hereinafter referred to as TiCO) layer and a carbonitride oxide (hereinafter referred to as TiCNO) layer and having an overall average layer thickness of 0.5 to 10 μm Compound layer,
(B) an α-type Al ₂ O ₃ layer having an average layer thickness of 1 to 15 μm as an upper layer;
There is known a coated cermet tool formed by vapor-depositing a hard coating layer composed of (a) and (b) above, and this coated cermet tool can be used for continuous cutting and intermittent cutting of various steels and cast irons, for example. It is well known to be used.

In general, the Ti compound layer and the α-type Al ₂ O ₃ layer constituting the hard coating layer of the above-mentioned coated cermet tool have a granular crystal structure, and further, the TiCN layer constituting the Ti compound layer is the layer itself. For the purpose of improving the strength of the crystal, a vertically grown crystal formed by chemical vapor deposition at a medium temperature range of 700 to 950 ° C. using a mixed gas containing an organic carbonitride as a reaction gas in a normal chemical vapor deposition apparatus. It is also known to have an organization.
Japanese Unexamined Patent Publication No. 6-31503 Japanese Patent Laid-Open No. 6-8010

In recent years, the use of FA for cutting devices has been remarkable. On the other hand, there has been a strong demand for labor saving and energy saving and further cost reduction for cutting work, and with this purpose, especially for the purpose of further extending the service life of cutting tools. upper layer constituting the hard coating layer, i.e. excellent but the hot hardness and thickening of one step in the α-type the Al ₂ O ₃ layer having heat resistance is strongly demanded, of the α-type the Al ₂ O ₃ layer When the layer thickness exceeds 15 μm, which is the maximum average layer thickness that has been practically used in the past, the Al ₂ O ₃ crystal grains become coarser and the denseness of the layer itself is significantly reduced. since the decrease in the high-temperature strength can not be avoided, the coated cermet tool formed by depositing formed as an upper layer of such thickening α type the Al ₂ O ₃ layer a hard coating layer, the thickening α-type Al ₂ O ₃ layer due to chipping to the cutting edge (fine Chipping) is likely to occur, since it becomes very short for this result useful life, it can not be put to practical use at present.

Therefore, the present inventors focused on the α-type Al ₂ O ₃ layer having an average layer thickness of 1 to 15 μm constituting the hard coating layer of the above-described conventional coated cermet tool from the above viewpoint, Research was conducted to develop a coated cermet tool in which chipping caused by the thickened α-type Al ₂ O ₃ layer does not occur at the cutting edge even if the layer thickness is increased to an average layer thickness exceeding 15 μm. result,
(A) Prior to the formation of the α-type Al ₂ O ₃ layer, which is the upper layer, on the surface of the tool base via the Ti compound layer, which is the lower layer of the hard coating layer, an ordinary chemical vapor deposition apparatus At
Under normal conditions, a TiCN layer is formed with an average layer thickness of 0.1 to 1 μm, and this is treated with a nitriding atmosphere treatment, preferably at a pressure of 20 to 40 kPa in a nitrogen atmosphere at a temperature of 950 to 1100 ° C. subjected to nitriding atmosphere under conditions of 60 minute hold, further followed by oxidation atmosphere treatment, is preferably gas composition, by _{volume%, CO 2: 5~10%,} CO: 5~10%, H 2: consisting of the remaining , Pressure: In an oxidizing atmosphere of 5 to 10 kPa, a Ti carbonitride oxide thin film (hereinafter referred to as a nuclear TiCNO thin film) is formed by performing an oxidizing atmosphere treatment at a temperature of 950 to 1100 ° C. for 3 to 10 minutes. In this state, when the α-type Al ₂ O ₃ layer is formed as an upper layer of the hard coating layer to a layer thickness of 16 to 30 μm exceeding the average layer thickness of 15 μm under normal conditions, the resulting nuclear TiCNO thin film Vapor deposition on top The thickened α-type Al ₂ O ₃ layer (hereinafter referred to as a thickened modified α-type Al ₂ O ₃ layer) was formed even though the average layer thickness was increased to a layer thickness of 16 to 30 μm. In addition, the coarsening of the Al ₂ O ₃ crystal grains is remarkably suppressed and the denseness of the layer itself is maintained, so that the high temperature strength is prevented from being lowered. The coated cermet tool, which is formed by vapor deposition in the state of coexisting with the Ti compound layer of the lower layer, with the α-type Al ₂ O ₃ layer as the upper layer of the hard coating layer, is superior in particular without chipping at the cutting edge. On the other hand, without forming the core TiCNO thin film, the normal condition, that is, the upper layer of the hard coating layer of the conventional coated cermet tool described above is exhibited. under the same conditions as the conditions for forming the mold the Al ₂ O ₃ layer, the average layer thickness 16 30μm of layer thickness in the formed thickened α type the Al ₂ O ₃ layer (hereinafter, referred to as a thick film normally α type the Al ₂ O ₃ layer) to a coated cermet tool formed by depositing formed as an upper layer of the hard coating layer, wherein Thickening Normal α-type Al ₂ O ₃ layer due to insufficient high-temperature strength, chipping occurs at the cutting edge, and the service life is reached in a short time.

(B) The above-mentioned thickened modified α-type Al ₂ O ₃ layer and the thickened normal α-type Al ₂ O ₃ layer are shown in FIGS. 1A and 1B using a field emission scanning electron microscope. As shown in the schematic explanatory diagram, each α-type Al ₂ O ₃ crystal grain having a hexagonal crystal lattice existing within the measurement range of the surface polished surface is irradiated with an electron beam, and the normal of the surface polished surface is Then, the inclination angle formed by the normal line of the (0001) plane, which is the crystal plane of the crystal grain, is measured, and the measurement inclination angle within the range of 0 to 45 degrees out of the measurement inclination angles is 0.25 degrees. In the case of creating an inclination angle number distribution graph that is divided for each pitch and totals the frequencies existing in each division, the thickened normal α-type Al ₂ O ₃ layer is as illustrated in FIG. , While the distribution of measured tilt angles on the (0001) plane shows an unbiased tilt angle number distribution graph within the range of 0 to 45 degrees. In the thickened modified α-type Al ₂ O ₃ layer, as illustrated in FIG. 2, at least two sharp peaks appear at specific positions in the tilt angle section, and these sharp peaks are shown on the horizontal axis of the graph. The positions and heights appearing in the inclination angle sections of the above change depending on the nitriding atmosphere processing conditions and the oxidizing atmosphere processing conditions when forming the above-described nuclear TiCNO thin film.

(C) According to the test results, in the above-described thickened modified α-type Al ₂ O ₃ layer, when forming the core TiCNO thin film, the nitriding atmosphere treatment and the oxidizing atmosphere treatment are performed under the conditions described above. In the inclination angle distribution graph of the thickening-modified α-type Al ₂ O ₃ layer, the highest peak is in the range of 7 to 15 degrees of the inclination angle section, and the second highest peak is 0 to 7 Appears within the range of degrees, and is the ratio of the entire frequency in the inclination angle distribution graph, and the total of the frequencies existing within the range of 7 to 15 degrees is 35% or more, within the range of 0 to 7 degrees An inclination angle frequency distribution graph in which the total number of frequencies present is 25% or more is displayed. Therefore, either the nitriding atmosphere treatment or the oxidizing atmosphere treatment is not performed under the above conditions, or the conditions of the treatment are the above If you deviate from the above conditions, In angle frequency distribution graph, now out of the range of frequency ratio with the inclination angle section and the inclination angle segment peak appears above, that this can not be obtained the desired effect of improving the high-temperature strength when.
The research results shown in (a) to (c) above were obtained.

The present invention has been made based on the above research results, and on the surface of a tool base composed of a WC-based cemented carbide or TiCN-based cermet,
(A) The lower layer is composed of one or more of a TiC layer, a TiN layer, a TiCN layer, a TiCO layer, and a TiCNO layer, all of which are formed by chemical vapor deposition, and a whole of 0.5 to 10 μm. A Ti compound layer having an average layer thickness;
(B) As an upper layer, each crystal grain having an α-type crystal structure in the state of chemical vapor deposition and having a hexagonal crystal lattice existing within the measurement range of the surface polished surface using a field emission scanning electron microscope Is irradiated with an electron beam to measure the inclination angle formed by the normal line of the (0001) plane, which is the crystal plane of the crystal grain, with respect to the normal line of the surface polished surface. A range of at least 7 to 15 degrees in an inclination angle distribution graph obtained by dividing the measured inclination angle within a range of ˜45 degrees into every 0.25 degree pitch and totaling the frequencies existing in each section. Of the frequency within the range of 7 to 15 degrees as a ratio to the total frequency in the inclination angle distribution graph. Total is 35% or more, 0-7 degrees The total of the frequencies present in the range of 25% or more, a is the inclination angle frequency distribution shows a graph, and thickening modified α type the Al ₂ O ₃ layer having an average layer thickness of 16～30Myuemu,
The hard coating layer formed by vapor deposition of the hard coating layer composed of (a) and (b) above is characterized by a coated cermet tool that exhibits excellent chipping resistance.

In addition, the reason why the numerical values of the constituent layers of the hard coating layer of the coated cermet tool of the present invention are limited as described above will be described below.
(A) Ti compound layer The Ti compound layer basically exists as a lower layer of the thickening-modified α-type Al ₂ O ₃ layer, and the high temperature strength of the hard coating layer is improved by its excellent high temperature strength. In addition to the tool substrate and the thickened modified α-type Al ₂ O ₃ layer, and thus has an effect of improving the adhesion of the hard coating layer to the tool substrate. If the thickness is less than 0.5 μm, the above-mentioned effect cannot be sufficiently exerted. On the other hand, if the average layer thickness exceeds 10 μm, the amount of thermoplastic deformation caused by heat generated during cutting increases beyond the allowable range. As a result, cracks are likely to occur in the thickened reformed α-type Al ₂ O ₃ layer, which is the upper layer, so the average layer thickness was determined to be 0.5 to 10 μm.

(B) Thickening-modified α-type Al ₂ O ₃ layer As described above, the thickening-modified α-type Al ₂ O ₃ layer has a tilt angle number distribution graph, and the highest peak is 7 in the tilt angle section. -15 degrees, and the second highest peak appears in each range of 0 to 7 degrees, and is a ratio of the entire frequency in the tilt angle frequency distribution graph of the frequencies existing in the range of 7 to 15 degrees. When the inclination angle number distribution graph in which the total is 35% or more and the total of the frequencies existing in the range of 0 to 7 degrees is 25% or more is shown, the average layer thickness may be increased to 16 to 30 μm. The high-temperature strength is maintained and chipping is suppressed. Combined with the excellent high-temperature hardness and heat resistance of the α-type Al ₂ O ₃ layer itself, long-term wear resistance of the hard coating layer Although it has the effect of contributing to the improvement of the properties, if the average layer thickness is less than 16 μm, it is necessary to increase the film thickness. It can not correspond to the partial satisfaction, whereas when the average layer thickness becomes too thick beyond 30 [mu] m, since the chipping is likely to occur, determined the average layer thickness and 16～30Myuemu.

  For the purpose of identification before and after the use of the coated cermet tool, a TiN layer having a golden color tone may be vapor-deposited as the outermost surface layer of the hard coating layer, but the average layer thickness in this case May be 0.1 to 1 μm, because if the thickness is less than 0.1 μm, a sufficient discrimination effect cannot be obtained, while the discrimination effect by the TiN layer is sufficient with an average layer thickness of up to 1 μm. .

In the coated cermet tool of the present invention, the thickened modified α-type Al ₂ O ₃ layer constituting the hard coating layer thereof has an inclination angle section within a range of at least 7 to 15 degrees as illustrated in FIG. In addition, there is a peak in the inclination angle section in the range of 0 to 7 degrees, and the total of the frequencies existing in the range of 7 to 15 degrees is 35% or more as a percentage of the entire frequency in the inclination angle distribution graph. , Showing an inclination angle number distribution graph in which the total of the frequencies existing in the range of 0 to 7 degrees is 25% or more, and even if the average layer thickness is increased to a layer thickness of 16 to 30 μm, excellent resistance is obtained. Since it exhibits chipping properties, it exhibits excellent wear resistance over a long period of time in the cutting of various steels and cast irons, enabling a further increase in service life.

  Next, the coated cermet tool of the present invention will be specifically described with reference to examples.

WC powder, TiC powder, ZrC powder, VC powder, TaC powder, NbC powder, Cr ₃ C ₂ powder, TiN powder, TaN powder, and Co powder all having an average particle diameter of 1 to 3 μm are prepared as raw material powders. These raw material powders were blended into the composition shown in Table 1, added with wax, ball milled in acetone for 24 hours, dried under reduced pressure, and pressed into a green compact with a predetermined shape at a pressure of 98 MPa. The green compact was vacuum sintered at a predetermined temperature in the range of 1370 to 1470 ° C. for 1 hour in a vacuum of 5 Pa. After sintering, the cutting edge portion was R: 0.07 mm honing By performing the processing, tool bases A to F made of a WC-base cemented carbide having a throwaway tip shape specified in ISO · CNMG120408 were manufactured.

In addition, as raw material powders, TiCN (mass ratio TiC / TiN = 50/50) powder, Mo ₂ C powder, ZrC powder, NbC powder, TaC powder, WC powder, all having an average particle diameter of 0.5 to 2 μm. Co powder and Ni powder are prepared, and these raw material powders are blended in the blending composition shown in Table 2, wet mixed by a ball mill for 24 hours, dried, and pressed into a compact at a pressure of 98 MPa. The green compact was sintered in a nitrogen atmosphere of 1.3 kPa at a temperature of 1540 ° C. for 1 hour, and after the sintering, the cutting edge portion was subjected to a honing process of R: 0.07 mm. Tool bases a to f made of TiCN-based cermet having a standard / CNMG12041 chip shape were formed.

Next, each of the tool bases A to F and the tool bases a to f was charged into a normal chemical vapor deposition apparatus. First, Table 3 (l-TiCN in Table 3 is disclosed in JP-A-6-8010). Tables 4 and 5 show the conditions for forming a TiCN layer having a vertically elongated crystal structure described below, and the other conditions for forming a normal granular crystal structure. A Ti compound layer having a target layer thickness to be deposited as a lower layer of a hard coating layer, and then, on the surface of the lower layer, first, a TiCN layer is deposited and formed under the conditions shown in Table 3,
(A) Pressure: In a nitrogen atmosphere of 25 kPa, a nitriding atmosphere treatment is performed at a temperature of 1000 ° C. for 10 to 60 minutes.
(B) Subsequently, the gas composition is in volume%, CO ₂ : 7%, CO: 7%, H ₂ : remaining, pressure: held in an oxidizing atmosphere of 7 kPa at a temperature of 1000 ° C. for 3 to 10 minutes. Applying an oxidizing atmosphere treatment under the conditions of
Similarly, a nuclear TiCNO thin film having a target layer thickness shown in Tables 4 and 5 is formed. In this state, the same conditions as those for forming the conventional α-type Al ₂ O ₃ layer shown in Table 3 are used. The coated cermet tools 1 to 13 of the present invention were produced by vapor-depositing a thickened modified α-type Al ₂ O ₃ layer having the target layer thickness shown as an upper layer of the hard coating layer.

For comparison purposes, as shown in Table 6, a thickened normal α-type Al ₂ O ₃ layer as an upper layer of the hard coating layer is shown in Table 3 without forming the above-described core TiCNO thin film. Comparative coated cermet tools 1 to 13 were respectively manufactured under the same conditions except that the film was formed under the same conditions as those for forming the conventional α-type Al ₂ O ₃ layer.

Thickened modified α-type Al ₂ O ₃ layer and thickened normal α-type Al ₂ O constituting the upper layer of the hard coating layer of the present invention coated cermet tool 1-13 and comparative coated cermet tool 1-13 _A tilt angle number distribution graph was created for each of the _three layers using a field emission scanning electron microscope.
That is, the inclination angle number distribution graph is set in a lens barrel of a field emission scanning electron microscope in a state where the surface of each of the various thickened α-type Al ₂ O ₃ layers is a polished surface. An electron backscattered diffraction image is obtained by irradiating an electron beam with an acceleration voltage of 15 kV at an incident angle of 70 ° to an individual crystal grain having a hexagonal crystal lattice existing within the measurement range of the surface polished surface with an irradiation current of 1 nA. Using an apparatus, an inclination angle formed by a normal line of the (0001) plane that is a crystal plane of the crystal grain with respect to a normal line of the surface-polished surface in a 30 × 50 μm region at an interval of 0.1 μm / step Based on the measurement result, the measurement inclination angle within the range of 0 to 45 degrees is divided into 0.25 degree pitches among the measurement inclination angles, and the frequency existing in each division is measured. Created by counting.

In the gradient angle distribution graphs of the various thickened α-type Al ₂ O ₃ layers obtained as a result, the inclination angle section showing the highest peak on the (0001) plane and the inclination angle section showing the second highest peak. Tables 4 to 6 show the ratios of the tilt angle numbers existing in the tilt angle section indicating the peak to the tilt angle number of the entire tilt angle number distribution graph, respectively.

In the gradient angle distribution graphs of the various thickened α-type Al ₂ O ₃ layers described above, as shown in Tables 4 to 6, the thickened modified α-type Al ₂ O ₃ layer of the coated cermet tool of the present invention. In any case, the peak of the distribution of the measured inclination angle of the (0001) plane appears in the inclination angle section within the range of at least 7 to 15 degrees and 0 to 7 degrees, and within the range of 7 to 15 degrees and 0 to 7 degrees. While the inclination angle number distribution graph in which the ratios of the inclination angle numbers existing in the inclination angle sections are 35% or more and 25% or more, respectively, the thickened normal α-type Al _{2 of the} comparative coated cermet tool is shown. All of the O ₃ layers have an unbiased distribution of measured inclination angles on the (0001) plane within a range of 0 to 45 degrees, no highest peak exists, and within a range of 7 to 15 degrees and 0 to 7 degrees. The ratio of the number of tilt angles existing in the tilt angle section is 20% or less in all cases. It was indicative of certain inclination angle frequency distribution graph.
Incidentally, FIG. 2, the inclination angle frequency distribution graph of the present invention the thickness of the coated cermet tool 2 form a film reformed α-type the Al ₂ O ₃ layer, FIG. 3, compare coated cermet tool 2 thickening normal α-type Al ₂ The graph of the distribution of the number of inclination angles of the O ₃ layer is shown respectively.

  Moreover, when the thickness of the constituent layer of the hard coating layer of the present invention coated cermet tools 1 to 13 and the comparative coated cermet tools 1 to 13 obtained as a result was measured using a scanning electron microscope (longitudinal section measurement) , Each showed an average layer thickness (average value of 5-point measurement) substantially the same as the target layer thickness.

Next, with the various coated cermet tools described above, the present coated cermet tools 1 to 13 and the comparative coated cermet tools 1 to 13 in a state where all of the various coated cermet tools are screwed to the tip of the tool steel tool with a fixing jig.
Work material: JIS / SNCM439 round bar,
Cutting speed: 220 m / min,
Cutting depth: 2mm,
Feed: 0.3mm / rev,
Cutting time: 20 minutes,
Dry continuous cutting test of alloy steel under the following conditions (referred to as cutting condition A),
Work material: JIS · S45C lengthwise equal 4 round grooved round bars,
Cutting speed: 250 m / min,
Incision: 1.5mm,
Feed: 0.35mm / rev,
Cutting time: 20 minutes,
Dry interrupted cutting test of carbon steel under the conditions (referred to as cutting condition B),
Work material: JIS / FCD550 round bar,
Cutting speed: 180 m / min,
Incision: 1.5mm,
Feed: 0.25mm / rev,
Cutting time: 20 minutes,
The dry continuous cutting test of cast iron was performed under the above conditions (referred to as cutting condition C), and the flank wear width of the cutting edge was measured in any cutting test. The measurement results are shown in Table 7.

From the results shown in Tables 4 to 7, the coated cermet tools 1 to 13 of the present invention are such that the upper layer of the hard coating layer has an inclination angle of (0001) plane of 7 to 15 degrees and 0 to 7 degrees. The highest peak and the second highest peak appear in the inclination angle sections of the above, and the total ratio of the frequencies existing in the inclination angle section ranges of 7 to 15 degrees and 0 to 7 degrees is 35% or more and 25, respectively. % Thick-type reformed α-type Al ₂ O ₃ layer showing an inclination angle number distribution graph that accounts for more than 15%, and cutting of steel and cast iron despite an average layer thickness of 16-30 μm The thickening-modified α-type Al ₂ O ₃ layer exhibits excellent chipping resistance, the occurrence of chipping at the cutting edge is remarkably suppressed, and excellent wear resistance is exhibited over a long period of time. The upper layer of the hard coating layer is (0 01) plane measured inclination angle distribution is unbiased manner in within the 0 to 45 degrees, compared to the highest peak is composed of a thicker usual α-type the Al ₂ O ₃ layer showing the inclination angle frequency distribution graph is not present In each of the coated cermet tools 1 to 13, when the above-mentioned thickened normal α-type Al ₂ O ₃ layer is thickened to an average layer thickness of 16 to 30 μm, the high-temperature strength is significantly reduced. It is clear that chipping occurs and the service life is reached in a short time.

As described above, the coated cermet tool according to the present invention can be used for various steels even when the α-type Al ₂ O ₃ layer, which is the upper layer of the hard coating layer, has an average layer thickness of 16 to 30 μm. It shows excellent chipping resistance in cutting work such as cast iron and cast iron, exhibits excellent wear resistance over a long period of time, and can extend the service life. It can cope with labor saving, energy saving and cost reduction of processing sufficiently satisfactorily.

It is a schematic diagram illustrating a measurement range of the inclination angle of the crystal grains (0001) plane in various thickened α type the Al ₂ O ₃ layer constituting the hard coating layer. It is an inclination angle number distribution graph of the (0001) plane of the thickening modified α-type Al ₂ O ₃ layer constituting the hard coating layer of the coated cermet tool 2 of the present invention. 4 is a graph showing the distribution of the number of inclination angles of the (0001) plane of the thickened normal α-type Al ₂ O ₃ layer constituting the hard coating layer of the comparative coated cermet tool 2.

Claims (1)

On the surface of the tool base composed of tungsten carbide based cemented carbide or titanium carbonitride based cermet,
(A) As a lower layer, each consists of one or more of a Ti carbide layer, a nitride layer, a carbonitride layer, a carbonate layer, and a carbonitride layer formed by chemical vapor deposition, and A Ti compound layer having an overall average layer thickness of 0.5 to 10 μm,
(B) As an upper layer, each crystal grain having an α-type crystal structure in the state of chemical vapor deposition and having a hexagonal crystal lattice existing within the measurement range of the surface polished surface using a field emission scanning electron microscope Is irradiated with an electron beam to measure the inclination angle formed by the normal line of the (0001) plane, which is the crystal plane of the crystal grain, with respect to the normal line of the surface polished surface. A range of at least 7 to 15 degrees in an inclination angle distribution graph obtained by dividing the measured inclination angle within a range of ˜45 degrees into every 0.25 degree pitch and totaling the frequencies existing in each section. Of the frequency within the range of 7 to 15 degrees as a ratio to the total frequency in the inclination angle distribution graph. Total is 35% or more, 0-7 degrees The total of the frequencies present in the range of 25% or more, a is the inclination angle frequency distribution shows a graph, and thickening modified α-type aluminum oxide layer having an average layer thickness of 16～30Myuemu,
A surface-coated cermet cutting tool that exhibits excellent chipping resistance with a thickened α-type aluminum oxide layer formed by vapor-depositing the hard coating layer composed of (a) and (b) above.

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