JP3252711B2 - Coated silicon nitride based tool - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a coated nitride comprising a substrate made of a silicon nitride ceramic in which at least a part of a grain boundary glass phase is crystallized, and a plurality of coating layers formed on the surface of the substrate. Silicon nitride-based tools are the most suitable as wear tools and cutting tools, especially as tools used for cutting, and have excellent coating layer exfoliation resistance, especially excellent wear resistance when cutting cast iron. It relates to a silicon-based tool.

[0002]

2. Description of the Related Art Tools using silicon nitride and sialon as a matrix have excellent toughness and thermal shock resistance as compared with conventional tools using alumina ceramics as a matrix. Further, since they are superior in heat resistance to coated carbide tools, they have come to be used as tools for high-speed cutting of cast iron irrespective of dry type or wet type. However, since silicon nitride has high reactivity with iron, its wear resistance is insufficient. Therefore, a coated silicon nitride-based tool coated with a ceramic layer such as a carbide or nitride of alumina or titanium has been proposed (Japanese Patent Application Laid-Open No. 56-1).
No. 6665, Japanese Patent Publication No. 61-19367).

[0003] However, these coated silicon nitride-based tools have succeeded in extending the tool life as compared with uncoated tools, but have insufficient adhesion strength between the silicon nitride and the coating layer. In addition, there has been a problem that the coating layer is apt to be peeled off and the variation in tool life becomes large. In addition, a chilled black scale exists on the surface of the cast iron,
The friction with the chill layer easily causes boundary wear at the cutting boundary of the tool, and there has been a problem that the size of the boundary wear is increased by performing the coating process. If the boundary wear increases, the quality of the work material decreases, or in extreme cases, the silicon nitride-based tool itself breaks, so reducing the boundary wear improves the performance of the coated silicon nitride-based tool. Has been one of the issues in doing so.

Here, boundary wear will be described with reference to the drawings. FIG. 1 is an enlarged perspective view schematically showing a corner portion of a tool tip as an example of a tool, and FIG.
It is a typical sectional view (B) along the XY direction of (A). With reference to FIGS. 1A and 1B, the corner portion of the tool tip includes a rake face 1 and a flank 2 and a cutting edge ridge A at a boundary between the rake face 1 and the flank 2. I have. With reference to FIG. 1 (C), the abrasion that occurs in the region indicated by 3 at the cutting edge ridge is referred to as boundary wear.

[0005] In order to suppress the occurrence of boundary wear as described above, attempts have been made to crystallize the grain boundary glass phase in the silicon nitride-based ceramics constituting the base of the tool. However, the present inventors have also found that, when the grain boundary glass phase is crystallized, there is a problem that the adhesion strength of the coating layer to the substrate is reduced and the wear resistance is reduced.

Some proposals have been made to improve the wear resistance by controlling the crystal particle diameter of the coating layer. For example, in Japanese Patent Publication No. 8-19525,
1-10μ with ceramics such as silicon nitride as base
A method for producing a tool in which titanium nitride or titanium carbonitride having a thickness of m is formed so as to cover the surface of a substrate by a suitable temperature chemical vapor deposition method and further coated with aluminum oxide and / or titanium nitride by a high temperature vapor deposition method has been proposed. I have.
However, in this proposal, since the thickness of the titanium nitride layer or the titanium carbonitride layer constituting the innermost coating layer is too large, it was not possible to sufficiently control the shape of the crystal grains constituting those layers. . Therefore, peeling or destruction of the coating layer easily occurs, and sufficient boundary wear resistance cannot be obtained.

[0007] Further, in Japanese Patent Application Laid-Open No. 5-208301, an average layer thickness of 0.
A base layer made of a titanium nitride layer having a thickness of 0.5 to 0.3 μm, and an average layer thickness of 0.1 to 0.4 μm formed on the base layer.
And an outermost layer formed of an aluminum oxide layer having an average grain size of 3 μm or less and an average layer thickness of 1.5 to 4.0 μm formed on the intermediate layer. A cutting tool made of coated silicon nitride-based ceramics characterized by this is proposed. However, in this proposal, the thicknesses of the underlayer and the intermediate layer are specified in order to make the average crystal grain size of the aluminum oxide layer 3 μm or less. The adhesion strength of the coating layer to a substrate, especially a silicon nitride-based ceramics substrate in which a grain boundary glass phase was crystallized, was insufficient. Furthermore, since the film quality of each layer constituting the coating layer, particularly the strength of the titanium compound-based coating layer, is insufficient, the boundary wear resistance cannot be sufficiently improved.

On the other hand, it is considered that an alumina film having excellent chemical stability to iron is indispensable as a coating layer in order to improve wear resistance in high-speed cutting of cast iron. Therefore, Japanese Patent Publication No. 59-13475 proposes to directly coat a silicon nitride base material with an alumina film. However, in this method, the alumina film grows abnormally, and the wear resistance and the peeling resistance are insufficient.

On the other hand, Japanese Patent Publication No. 61-19367 discloses that an alumina film is coated with a compound film such as Ti, Zr or the like to suppress abnormal grain growth of alumina, and to provide abrasion resistance and peeling resistance. Techniques for improving the performance have been proposed. However, even in this proposal, the properties of the alumina crystal grains were not sufficiently controlled, and the wear resistance, particularly the boundary wear resistance, could not be sufficiently improved.

Accordingly, an object of the present invention is to provide a coated silicon nitride-based tool capable of improving the adhesion strength of a coating layer to a substrate, improving the boundary wear resistance, and stabilizing the tool life. It is.

[0011]

Means for Solving the Problems The present inventors have conducted various studies and studied the mechanism of boundary wear generation of a coated silicon nitride based tool. As a result, in the conventional coated silicon nitride-based tool, the coating layer having low adhesion strength is easily peeled off by the chilled black scale, and the peeled coating layer becomes hard wear powder, and the silicon nitride-based tool is removed. It was thought that the material penetrated between the substrate made of ceramics and the black scale, abrasively abraded the substrate made of silicon nitride ceramics, and the amount of boundary wear would be larger than that of a tool not coated.

Further, the present inventors have found that the above-mentioned peeling phenomenon depends not only on the simple adhesion strength between the substrate and the coating layer but also on the strength of the coating layer itself. Therefore, the present inventors considered that if a coating layer that is difficult to peel off and has excellent strength can be formed on a substrate made of a silicon nitride-based ceramic, coarsening of boundary wear can be suppressed.

Next, when a coating layer is formed on a silicon nitride ceramic in which at least a part of the grain boundary glass phase is crystallized, the coating layer is formed on the silicon nitride ceramic in which the grain boundary glass phase is not crystallized. The present inventors have studied the cause of the decrease in adhesion strength as compared with the case of forming. As a result, when the grain boundary glass phase is not crystallized in the silicon nitride-based ceramic, nucleation sites of crystals constituting the coating layer are preferentially formed in the grain boundary glass phase, and the adhesion of the coating layer to the substrate is reduced. When the grain boundary glass phase was crystallized while the strength could be ensured, it was considered that the nucleation sites were reduced and the adhesion was reduced.

Therefore, the present inventors have further studied and found that the grain size and shape of the crystal grains constituting the coating layer are finely controlled in the initial stage and the later stage of the coating layer formation.
A coating layer having excellent peeling resistance and adhesion strength can be formed on a substrate made of a silicon nitride-based ceramic in which at least a part of the grain boundary glass phase is crystallized. It has been found that a coating layer having excellent boundary wear can be formed.

Based on the above findings, the coated silicon nitride-based tool according to the present invention provides a substrate made of a silicon nitride-based ceramic in which at least a part of a grain boundary glass phase is crystallized, A coated silicon nitride-based tool comprising a plurality of formed coating layers, wherein the innermost coating layer adjacent to the substrate includes columnar crystals having an average crystal grain width of 5 to 100 nm, and a thickness of 0.1 to 0.7 μm. It is a titanium nitride layer having a thickness.

The innermost coating layer may be a substrate
At least a portion of the titanium nitride layer adjacent to the
Includes granular crystals having a crystal grain size of 1 to 30 nm. Of titanium nitride layer
Preferably the thickness is in the range of 0.3-0.5μm
No.

Further, the coating layer includes a single alumina layer, which is formed directly on the outside of the titanium nitride layer and has an average crystal grain size of 50 to 500 nm.
It is preferable to include m crystal grains.

Further , at least a part of the surface of the coating layer is
It is preferable that the coating layer has a surface area enlarged at a ratio of 1.01 to 1.03 with respect to a mirror surface area of at least a part of the coating layer . In this case, the overall thickness of the coating layer is 1
It is preferably about 2 μm.

Preferably, at least a part of the crystallized grain boundary glass phase contains at least one of Y ₂ SiO _{7 and} YAlO ₃ .

In at least a part of the working part of the tool , a coating layer may be formed on a substrate that has not been subjected to a grinding treatment.

[0021]

BEST MODE FOR CARRYING OUT THE INVENTION In the coated silicon nitride-based tool of the present invention, the innermost coating layer adjacent to the substrate contains columnar crystals having an average crystal grain width of 5 to 100 nm, and has a thickness of 0.1 to 0.1 nm.
It is a titanium nitride layer having a thickness of 0.7 μm. By configuring the titanium nitride layer, which is the innermost coating layer, as described above, at the time of cutting cast iron, it is possible to prevent the coating layer from being broken by the black skin portion of the cast iron, which is chilled and has a higher hardness. In addition, excellent adhesion to a substrate made of a silicon nitride ceramic in which at least a part of the grain boundary glass phase is crystallized can be ensured.

Here, the average crystal grain width of the columnar crystals is 5 nm.
It is industrially difficult to make it smaller than 100 n
When it is larger than m, the boundary wear resistance is reduced. If the thickness of the titanium nitride layer is smaller than 0.1 μm, a portion where the surface of the substrate is not locally covered by the coating layer occurs. Even if the thickness of the titanium nitride layer is larger than 0.7 μm, it causes a decrease in the boundary wear resistance. For these reasons, the average crystal grain width of the columnar crystals and the thickness of the titanium nitride layer were limited to the above ranges.

In the case where a coating layer is formed on the surface of the substrate without grinding treatment in at least a part of the operating portion of the surface of the substrate made of the silicon nitride ceramics, Therefore, a portion not covered by the titanium nitride layer is likely to be generated. In consideration of such a case, the particularly preferable thickness of the titanium nitride layer is in the range of 0.3 to 0.5 μm.

In order to form a titanium nitride layer having the above structure, at least the temperature at the start of coating (start temperature at the time of forming the coating layer) is preferably lower than 950 ° C., more preferably. Is desirably a temperature lower than 900 ° C.

Further, the innermost coating layer is adjacent to the substrate.
At least a part of the contacting portion of the titanium nitride layer includes a granular crystal having a crystal grain size of 1 to 30 nm, and a columnar shape having an average crystal grain width of 5 to 100 nm from the granular crystal having a crystal grain size of 1 to 30 nm from the substrate side to the outer surface. By having a structure that changes to a crystal, particularly excellent adhesion strength of the coating layer, abrasion resistance,
Shows boundary wear resistance. As described above, in order to generate a granular crystal at a portion adjacent to the substrate made of silicon nitride ceramics, that is, at an interface with the substrate, for example, the furnace pressure in the initial stage of forming the coating layer is set to a low pressure of 50 Torr or less. Then, it is necessary to change the furnace pressure to about 100 Torr. Here, the average crystal particle diameter of the granular crystals is 1n.
Making it smaller than m has little industrial significance.
If it is larger than 30 nm, the boundary wear resistance is reduced. For such a reason, the range of the crystal particle diameter of the portion adjacent to the base was set.

Further, it is preferable that the coating layer constituting the coated silicon nitride-based tool of the present invention contains at least one alumina layer. When this alumina layer is formed directly on the outer side of the titanium nitride layer, the crystal grains of titanium nitride are very fine, and the surface of the titanium nitride layer is flat. The formation is very dense and uniform. In particular, when the average crystal grain size of alumina constituting the alumina layer is in the range of 50 to 500 nm, the surface becomes very fine and has a small surface roughness, the adhesion strength to the titanium nitride layer is improved, and the fracture strength of the alumina layer is improved. Therefore, wear resistance and chipping resistance, particularly boundary wear resistance, are improved.

The alumina layer is most preferably formed directly on the titanium nitride layer located on the innermost side of the coating layer. However, it is preferably 0 if the effect of the fine titanium nitride particles is not reduced. A layer of a titanium-based compound having a thickness of 0.5 μm or less, more preferably, a layer of a titanium-based compound having a thickness of 0.3 μm or less may be formed between the titanium nitride layer and the alumina layer. In this case, examples of the titanium-based compound include titanium carbide, carbonitride, boronitride, carbonate, and carbonitride.

As the crystal phase of alumina constituting the above-mentioned alumina layer, κ-alumina showing fine film quality is preferable, but as long as the effects of the present invention are achieved,
α-alumina may be used.

Further, a layer having a low coefficient of friction, for example, a titanium nitride (TiN) layer may be formed as the outermost layer of the coating layer in order to improve the chip discharge property.

Further, the present inventors have proposed that at least
A part of the surface has a surface area enlarged at a certain ratio with respect to a surface area of at least a part of a mirror state of the coating layer, so that peeling resistance and fracture resistance of the coating layer can be improved. Was found. Based on such knowledge, in the coated silicon nitride based tool according to the present invention,
At least a part of the coating layer has at least one of the coating layers.
It has an enlarged surface area at a ratio in the range of 1.01 to 1.03 with respect to the mirror surface area of the portion . At this time, it is preferable that the entire film thickness of the above-mentioned coating layer is in the range of 1 to 2 μm. It is preferable that at least a part of the coating layer is a cutting edge ridge portion, a rake face, or a flank area of the tool.

The above enlargement ratio is specifically measured by the following method as an example. The above enlargement ratio is measured as the increase surface area ratio, in other words, the less the covering layer
At least some of the surfaces are measured as an increased surface area ratio of 1-3%. As an example of the increased surface area ratio, a value measured using a three-dimensional roughness profile measuring device manufactured by Elionix Inc. is used. The magnification is set to 5000 times to measure the surface of the coating layer, and the sampling numbers in the horizontal and vertical directions in the measurement visual field are set to 280 points and 210 points, respectively. Here, assuming that the area of the measurement visual field is Sm and the surface area of the measured portion is Sa, the increase surface area ratio ΔS is expressed by the following equation.

ΔS = (Sa / Sm−1) × 100 (%) The numerical value quantified by the above equation is defined as the increased surface area ratio. If the device can be measured by the same principle, the quantified numerical value can be used for the same index. In this case, the measured visual field surface area Sm corresponds to the specular surface area of the coating layer, and the measured surface area Sa corresponds to the measured visual field area Sm and corresponds to the enlarged surface area of the coating layer.

In the above measurement, the measurement magnification is
In order to eliminate undulations on the surface of the substrate on which the coating layer is formed and to measure fine irregularities, for example, it is set to 5000 times.

Using the index as described above, the surface roughness in the height direction, which has been noticed conventionally, for example, Ra, Rma
It is possible to obtain not only information on surface roughness such as x but also information on three-dimensional surface roughness including information on surface roughness in the horizontal direction. Furthermore, with a conventional stylus-type roughness measuring instrument, a stylus cannot be inserted into a concave portion of an unevenness of a coating layer having fine crystal particles having a particle diameter of 50 to 500 nm, so that a coating layer having fine unevenness is formed. Could not be quantified. However, in this measurement using an electron beam, it is possible to measure the shape of even a very narrow portion where the interval between the concave portions is 500 nm or less, so that the surface of a material having a very fine concave portion such as a coating layer can be measured. Suitable for evaluating properties. Even if the coating layers have the same average crystal grain size, the ratio of the increased surface area may be significantly different. The present inventors have paid attention to this fact, and have found that particularly when the increased surface area ratio is 1 to 3%, excellent wear resistance and boundary wear resistance are exhibited.

If the total thickness of the coating layer is smaller than 1 μm, the effect provided by the coating layer is small, and
If it is thicker, it becomes difficult to keep the increased surface area ratio within the range of 1 to 3%. Therefore, the total thickness of the coating layer is limited to the above range.

The silicon nitride ceramic used as a substrate in the coated silicon nitride tool of the present invention includes:
The one in which at least a part of the grain boundary glass phase is crystallized is used. When at least one of Y ₂ SiO ₇ or YAlO ₃ is contained as a component of the crystallized grain boundary phase, compared with the case where other crystal phases are precipitated at the grain boundary,
The adhesion strength of the coating layer to the substrate is increased, and the boundary wear resistance is excellent.

Since machining of silicon nitride ceramics is difficult, the grinding cost tends to be higher than other tool materials. For this reason, attempts have been made to use the silicon nitride-based ceramic as a tool without grinding the surface of the silicon nitride-based ceramic used as a substrate. However,
In silicon nitride, β-silicon nitride that grows in a needle shape during sintering easily grows freely on the surface. If a coating layer is formed on a sintered body having such a surface without grinding, the β-silicon nitride that has grown freely grows. -It is known that crystal nuclei constituting the coating layer are preferentially generated at the tip of silicon nitride, and abnormal grain growth occurs. Although some proposals have been made to prevent such a phenomenon, fine recesses are present on the surface of the silicon nitride-based ceramics sintered body that has not been subjected to the grinding treatment, and the crystal constituting the coating layer is formed. Nuclei are still insufficient to form in these recesses. For this reason, the adhesion strength of the coating layer to the substrate becomes insufficient, and thus improvement in peel resistance has been desired.

In order to solve such a conventional problem, when a very fine titanium nitride layer as in the present invention is formed as the innermost layer adjacent to the substrate, the silicon nitride ceramic sintered body constituting the substrate is formed. It has been found that nuclei of the titanium nitride layer are also generated in the concave portions on the surface of the above, and the adhesion strength of the coating layer is dramatically improved. Thus, a high-performance and inexpensive coated silicon nitride-based tool can be manufactured. The industrial value of this is enormous.

[0039]

【Example】

(Example 1) Using a ball mill lined with alumina, 93% by weight of α-silicon nitride powder and 2% of alumina powder were used.
5% by weight of yttria powder was mixed in ethanol at a ratio of 5% by weight, and the mixed powder was granulated by a spray drier. The powder thus treated was pressed with a mold at a pressure of 1 ton / cm ² . The obtained molded body was placed in a nitrogen gas at 5 atm and a temperature of 1800 ° C. for 1 hour.
Hold for a time and sinter. Further, the sintered body is heat-treated while being held at a temperature of 1400 ° C. for 4 hours in a nitrogen gas,
The grain boundary glass phase was crystallized.

Next, the upper and lower surfaces of the obtained silicon nitride-based ceramics sintered body are ground, and after the outer periphery is ground, a cut where the rake face 1 and the flank 2 intersect as shown in FIG. Chamfering was performed so that the angle θ was 25 ° and L was 0.2 mm at the blade ridge line portion. Thus, IS
An O-shaped SNGN120408-shaped chip was produced.
When the crystal phase of this chip was examined using X-ray diffraction by Cu-Kα ray, YNS was determined as a crystallized glass phase.
iO ₂ and Y ₂ Si ₃ N ₄ O ₃ were observed.

The nitrogen prepared as the chip thus prepared is
The surface of the silicon carbide ceramic sintered body
Using a chemical vapor deposition apparatus, H_Two, N_Two, Ti
Cl _FourAt a furnace pressure of 100 Torr by using
It was formed so as to cover the coating layer. Note that the titanium nitride layer
The forming temperature (coating temperature) is as shown in Table 1. Further
H as the upper layer_Two, CO_Two, AlCl
_Three, H_TwoS at a furnace pressure of 100 Torr
An alumina layer with a thickness of 1 μm at a temperature of 1000 ° C. and a titanium nitride layer
Sample N shown in Table 1
o. 1-1 to 1-8 were prepared.

Tomographic images of these samples were photographed with a transmission electron microscope at a magnification of 60,000 to 700,000, and the average crystal grain width of the titanium nitride layer and the average crystal grain diameter of the alumina layer were measured. The average crystal grain width or average crystal grain diameter is obtained by drawing a straight line that crosses the cross-sectional shape of each of several crystal grains, and determining the distance between two points where the straight line and the cross-sectional outline of the crystal grain intersect. The particle diameter was measured and their average was measured. The crystal grain width of the columnar particles in the titanium nitride layer was determined by drawing a straight line at the approximate center of the particle in the thickness direction of the titanium nitride layer, and using the distance between two points where the straight line intersected the outer shape of the particle. .

Next, a test was performed to determine the load (peeling load) when peeling occurred in the coating layer by a method in which a diamond Vickers indenter was pressed against the surface of these samples from the vertical direction and the sample was scratched while applying a constant load. Done.

A cast iron (FC25) with black scale was cut at a cutting speed of 500 m / min. , Feed 0.3mm / re
v. The wafer was cut for 10 minutes by a wet method with a cut of 1.5 mm, and the average amount of wear on the flank and the amount of boundary wear were measured.

The above measurement results are shown in Table 1.
In Table 1, the sample No. The sample in which * is added to the right shoulder of the numeral indicating that this is an example of the present invention.

As can be seen from Table 1, when the titanium nitride layer as the innermost layer adjacent to the surface of the silicon nitride ceramic sintered body is mainly composed of columnar crystals having an average crystal grain width of 5 to 100 nm, The average crystal particle diameter of the alumina layer can be as small as 50 to 500 nm, the adhesion strength of the coating layer,
It turns out that it is excellent in abrasion resistance and peeling resistance. Also,
It can be seen that when the thickness of the titanium nitride layer is 0.3 to 0.5 μm, a coated silicon nitride-based tool having particularly excellent boundary wear resistance can be obtained.

(Example 2) When a titanium nitride layer is formed on the surface of a substrate made of the same silicon nitride-based ceramics sintered body as used in Example 1 so as to cover an adjacent innermost layer. During the first 10 minutes of the forming process (only one sixth of the time for forming the titanium nitride layer), the sample pressure was set to 20 Torr, except that the sample pressure was 20 Torr. 1
Sample N shown in Table 1 under the same coating layer formation conditions as
o. 2-1 was produced.

When the coating layer of this sample was observed with a transmission electron microscope at a magnification of 60,000 to 700,000, the crystal grain size was found near the interface between the substrate made of silicon nitride ceramic and the titanium nitride layer. Granular crystals of ３０30 μm were observed. In the same manner as in Example 1, the peeling load, the average flank wear, and the boundary wear measured in order to evaluate the adhesion strength and wear resistance of the coating layer of this sample are shown in Table 1. According to the results, the sample N having granular crystals near the interface between the substrate made of silicon nitride ceramics and the titanium nitride layer
o. Sample No. 2-1 does not include granular crystals. 1
It can be seen that the adhesive strength and abrasion resistance are superior to -4.

[0049]

[Table 1]

Example 3 As shown in Table 2, substrates (base materials) (A to E) made of silicon nitride ceramic sintered bodies having various grain boundary crystal phases were prepared. A has the same composition as that of the substrate produced in Example 1 and has not been subjected to heat treatment for crystallizing at least a part of the grain boundary glass phase;
B is obtained by subjecting A to HIP (hot isostatic pressing) in a nitriding gas at a temperature of 1700 ° C. and 1000 atm.

The sample No. prepared in Example 1 was applied to these substrates. 1-1 and No. 1 The same coating layer as in 1-4 was formed, and the peeling load was measured as the adhesion strength in the same manner as in Example 1, and the average flank wear and boundary wear were measured as the evaluation of wear resistance. The results are shown in Table 3. In Table 3, “a” is the sample No. as the coating layer type.
1-1 shows that the coating layer is the same as that of Sample No. 1-1. It shows that it is the same coating layer as 1-4. Further, in Table 3, the sample No. The ones with asterisks on the right shoulder of the numbers indicating are examples of the present invention.

Referring to Tables 1 and 3, sample no. 3
-1 and No. 1-1, No. 1; According to the comparison of 3-3, in the sample in which the coating layer (a) having a configuration different from that of the present invention was formed, the sample in which the grain boundary glass phase was crystallized was better than the sample in which the grain boundary glass phase was not crystallized. It can be seen that the adhesion strength has decreased. Sample N
o. 3-2 and no. 1-4, No. According to the comparison of 3-4, in the sample in which the coating layer (b) having the configuration of the present invention was formed, the sample in which the grain boundary glass phase was crystallized had the same or higher adhesion than the sample in which the grain boundary glass phase was not crystallized. It turns out that it has strength.

In each of the samples subjected to the crystallization treatment of the grain boundary phase, the sample provided with the coating layer (b) having the structure of the present invention has a coating layer ( It can be seen that the adhesive strength and the cutting performance, that is, the abrasion resistance, are superior to those of the case a). Among them, Sample No. 1 having Y ₂ SiO ₇ and YAlO ₃ as the grain boundary crystal phase exhibits particularly excellent performance. 3-6.

[0054]

[Table 2]

[0055]

[Table 3]

(Example 4) The rake face of the sample prepared in Example 1 was measured at a magnification of 5000 times using a three-dimensional shape measuring device manufactured by Elionix Inc. (model number ERA-8000), and the increased surface area ratio was determined. Was. Table 4 shows the results. In Table 4, sample No. The ones with an asterisk on the right shoulder of the number indicating the present invention indicate examples of the present invention.

As can be seen from Tables 1 and 4, the sample N of the present invention having an increased surface area ratio in the range of 1 to 3% was used.
o. It turns out that 1-3, 1-4, and 2-1 show especially excellent boundary wear resistance. Sample No. of the present invention example. 1-6
Was very fine and preferable in terms of the average particle width of the titanium nitride layer and the average particle diameter of the alumina layer. According to the macroscopic surface roughness observation using the above-described measuring device, the surface was locally coarse. It is considered that the increased surface area ratio was increased due to the generation of the fine alumina particles, and the boundary wear amount became a slightly large value. The reason for the formation of the alumina layer having such coarse particles is that the thickness of the titanium nitride layer as the inner layer was too thin as 0.1 μm, and that the base layer not locally covered by the titanium nitride layer was used. Since a surface portion is formed and the alumina layer directly covers the substrate made of the silicon nitride ceramics at that portion, it is considered that abnormal grain growth of alumina has occurred.

[0058]

[Table 4]

(Example 5) The sample no. Sample No. 2-1 differs only in the thickness of the alumina layer from Sample No. 2-1. 5-1, 5-2, and 5-3 were produced. Using these samples, the adhesion strength and the cutting performance (wear resistance) were evaluated in the same manner as in Example 1, and the measurement results of the peel strength, the flank average wear amount, and the boundary wear amount are shown in Table 5. Table 5 also shows the results of the increased surface area ratio measured in the same manner as in Example 4.

As can be seen from Table 5, the samples having an overall coating layer thickness of 2 μm or less have an increased surface area ratio of 3% or less and a small amount of boundary wear.

[0061]

[Table 5]

(Example 6) A substrate having the same composition as the substrate (C) made of the silicon nitride-based ceramics produced in Example 3 was subjected to overall grinding (grip of the rake face and flank face).
A chip having the shape of SO model number SNGN120408 and an ISO model number SNMN1204 in which only the rake face is ground.
A chip having a shape of 08 was produced. In addition, as shown in FIG. 1B, the angle θ is 25 ° at the cutting edge ridge portion where the rake face 1 and the flank face 2 intersect as shown in FIG.
And the length L was 0.2 mm.

The sample No. prepared in Example 1 was placed on the surface of the substrate of these chips. A coating layer having the same configuration as that of 1-1 and 1-4 was formed, and the same cutting test as in Example 1 was performed to evaluate the cutting performance (wear resistance).

Table 6 shows the results. In Table 6, “a” is the sample No. as the coating layer type. 1-1
Indicates that the coating layer has the same configuration as “b”.
Is the sample No. It shows that the coating layer has the same configuration as 1-4. In addition, the sample No. A number with asterisks at the right shoulder of the numerical value indicating that this is an example of the present invention. Further, in the presence or absence of an unground surface, “none” indicates that the entire surface including the rake surface and the flank surface has been ground, and “present” indicates that only the rake surface has been ground.

As can be seen from Table 6, the sample No. in which the coating layer (a) having a configuration different from that of the present invention was formed on the surface of the chip base having only the rake face ground. In 6-3, peeling of the coating layer occurred early, and the amount of boundary wear showed a large value. Further, Sample No. 1 in which the coating layer (b) having the configuration of the present invention was formed on the surface of the chip base having only the rake face ground. In Sample No. 6-4, Sample No. 6 in which the coating layer (b) having the structure of the present invention was formed on the surface of the chip substrate that had been entirely ground. Cutting performance (abrasion resistance) almost equivalent to that of 6-2 was able to be realized.

[0066]

[Table 6]

The embodiments and examples of the invention disclosed above are to be considered in all respects as illustrative and not restrictive. The scope of the present invention is defined by the terms of the claims, rather than the description above, and is intended to include any modifications within the scope and meaning equivalent to the terms of the claims.

[0068]

As described above, according to the present invention, in a silicon nitride based tool having a coating layer formed thereon, the coating layer can have improved peeling resistance and wear resistance, particularly, boundary wear resistance. As a result, it becomes possible to remarkably stabilize the tool life at the manufacturing site of machining at the industrial level, in which the coated silicon nitride-based tool is used.

[Brief description of the drawings]

FIG. 1A is a perspective view schematically showing a corner portion of a tool tip as an example of a tool according to the present invention in an enlarged manner, and FIG. 1B is a schematic cross-sectional view taken along the X-Y direction in FIG. FIG. 4 is a perspective view (C) showing a portion where boundary wear occurs.

[Explanation of symbols]

 1 Rake face 2 Flank face 3 Boundary wear A Cutting edge ridge

──────────────────────────────────────────────────続 き Continued on front page (58) Field surveyed (Int.Cl. ⁷ , DB name) B23B 27/14 C23C 16/34

Claims (7)

(57) [Claims] 1. A coated silicon nitride-based tool comprising: a base made of a silicon nitride-based ceramic in which at least a part of a grain boundary glass phase is crystallized; and a plurality of coating layers formed on a surface of the base. The innermost coating layer adjacent to the substrate contains columnar crystals having an average crystal grain width of 5 to 100 nm, and 0.1 to 0.1 nm.
A titanium nitride layer having a 0.7μm thickness, the group
At least a portion of the titanium nitride layer adjacent to the body
Is a coated silicon nitride-based tool, characterized by containing granular crystals having a crystal grain size of 1 to 30 nm . 2. The titanium nitride layer having a thickness of 0.3 to 0.1.
The coated silicon nitride-based tool according to claim 1, wherein the thickness is 5 µm. 3. The coating layer includes at least one alumina layer, the alumina layer being formed directly on the outside of the titanium nitride layer, and having an average crystal grain size of 50 to 50.
2. The method according to claim 1 , further comprising a crystal grain of 0 nm.
A coated silicon nitride-based tool according to claim 2 . 4. The method according to claim 1, wherein at least a part of the surface of the coating layer is
4. The coating layer according to claim 1 , wherein the coating layer has a surface area enlarged at a ratio of 1.01 to 1.03 with respect to a mirror surface area of at least a part of the coating layer.
2. The coated silicon nitride-based tool according to claim 1. 5., wherein the thickness of the whole of the coating layer is 1 to 2 [mu] m, coated silicon nitride tool according to claim 4. 6. At least a portion of the grain boundary glass phase that the crystallization, characterized in that it comprises at least one selected from the group consisting of Y ₂ SiO ₇ and YAlO _3, wherein
The coated silicon nitride-based tool according to any one of claims 1 to 5 . In 7. At least a part of the operation of the tool, wherein the coating layer on the substrate grinding process is not applied is formed, 請claim 1
Coated silicon nitride tool according to any one of up to Motomeko 6.