WO2015097856A1 - サイアロン焼結体及び切削インサート - Google Patents
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- WO2015097856A1 WO2015097856A1 PCT/JP2013/085085 JP2013085085W WO2015097856A1 WO 2015097856 A1 WO2015097856 A1 WO 2015097856A1 JP 2013085085 W JP2013085085 W JP 2013085085W WO 2015097856 A1 WO2015097856 A1 WO 2015097856A1
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- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23B—TURNING; BORING
- B23B27/00—Tools for turning or boring machines; Tools of a similar kind in general; Accessories therefor
- B23B27/14—Cutting tools of which the bits or tips or cutting inserts are of special material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D18/00—Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for
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Definitions
- This invention relates to a sialon sintered body and a cutting insert.
- the sialon sintered body is recognized as a material having excellent hardness compared to silicon nitride and high strength in a temperature range from room temperature to high temperature and high chemical stability. Accordingly, the sialon sintered body is expected to be used in a wide range of applications such as machine parts, heat-resistant parts, and wear-resistant parts.
- One application of the sialon sintered body is a cutting insert attached to a cutting tool (for example, Patent Documents 1 to 5).
- the cutting insert is a cutting edge that is detachably attached to the tip of the main body of the cutting tool, and is a tool component that is also referred to as a throw-away tip, a cutting edge replacement tip, or the like.
- JP 2008-162882 A JP 2013-224240 A WO2010 / 103839A1 JP 60-239365 A Special table 2008-529948
- An object of the present invention is to provide a sialon sintered body and a cutting insert having fracture resistance, VB wear resistance, and boundary wear resistance.
- a sialon sintered body comprising ⁇ -sialon and at least one polytype sialon selected from the group consisting of 12H-sialon, 15R-sialon, and 21R-sialon, Z value of ⁇ -sialon represented by Si 6-Z Al Z O Z N 8-Z is 0.4 or more and 1.0 or less, Percentage of the total I p of the peak intensity of each polytype sialon calculated from the peak intensity of the polytype sialon to the total I A of the peak intensity of each sialon calculated from the peak strength of the obtained sialon by X-ray diffraction analysis [ (I p / I A ) ⁇ 100] is 10% or more and 50% or less, At least one rare earth element B selected from the group consisting of La and Ce, and at least one rare earth element C selected from the group consisting of Y, Nd, Sm, Eu, Gd, Dy, Er, Yb, and Lu; Including
- the ratio [(I ⁇ / I A ) ⁇ 100] of the peak intensity I ⁇ of ⁇ -sialon to the total I A of the peak intensity of each sialon obtained by X-ray diffraction analysis is less than 10%
- M is a metal element containing the rare earth element B and the rare earth element C
- the ratio A ⁇ / A S of the atomic ratio A ⁇ of the rare earth element B to the rare earth element C in the ⁇ -sialon to the atomic ratio A S of the rare earth element B to the rare earth element C in the sialon sintered body is 70% or less.
- the sialon sintered body according to [1] or [2].
- the sialon sintered body according to the present invention has fracture resistance, VB wear resistance, and boundary wear resistance. Moreover, since the cutting insert according to the present invention is made of a sialon sintered body having fracture resistance, VB wear resistance, and boundary wear resistance, rough machining is performed when cutting a work material such as a heat resistant alloy. It is possible to exhibit sufficient cutting performance over a long period of time in both the intermediate finishing and the intermediate finishing. Therefore, according to the present invention, it is possible to provide a long-life cutting insert that can be used for both roughing and intermediate finishing when a work material such as a heat-resistant alloy is cut.
- FIG. 1 is a schematic explanatory view showing an embodiment of the cutting insert of the present invention.
- FIG. 2 is a schematic explanatory view showing an embodiment of a cutting tool provided with the cutting insert shown in FIG.
- the sintered sialon of the present invention contains ⁇ -sialon and at least one polytype sialon selected from the group consisting of 12H-sialon, 15R-sialon, and 21R-sialon.
- ⁇ -sialon usually has a needle-like form. Therefore, when a large amount of ⁇ -sialon is present in the sialon sintered body, a structure in which needle-like crystal grains are intertwined in a complex manner is formed, and the progress of cracks in the sialon sintered body due to external stress is suppressed. Is done. That is, as the proportion of ⁇ -sialon in the sialon sintered body increases, the fracture resistance of the sialon sintered body improves.
- the sialon sintered body only needs to have at least one of these.
- 12H-sialon is preferred in terms of a good balance between fracture resistance and wear resistance.
- the sialon sintered body of the present invention preferably contains ⁇ -sialon and polytype sialon in a total of 70 area% or more and 98 area% or less, and 85 area% or more and 97 area% or less with respect to the sialon sintered body. Is more preferable. If ⁇ -sialon and polytype sialon are contained in the sialon sintered body at the above ratio, the characteristics of ⁇ -sialon and polytype sialon are easily reflected as the characteristics of the sialon sintered body. Thus, the phase which determines the characteristic of a sialon sintered compact may be called a main phase. Therefore, if ⁇ -sialon and polytype sialon are contained in the above ratio, desired performance can be obtained.
- hard carbonitrides such as SiC, TiN, TiCN, TiC, and WC may be included in addition to the main phase.
- ⁇ -sialon and polytype sialon contained in the sialon sintered body at the above ratio are crystal grains having a minor axis diameter of submicron to several microns and an aspect ratio of about 1 to 20 in the sialon sintered body. Often exists.
- a grain boundary phase that is amorphous or partially crystalline exists between the crystal grains. The grain boundary phase exists as a liquid phase during the sintering of the sialon sintered body and contributes to the improvement of the sinterability of the sialon sintered body.
- the total amount of ⁇ -sialon and polytype sialon with respect to the sialon sintered body can be obtained as follows.
- the sialon sintered body is cut at an arbitrary plane, and the mirror-cut cut surface is photographed with a scanning electron microscope at a magnification of 2000 to 5000 times.
- the obtained microstructure photograph is subjected to image analysis to classify ⁇ -sialon and polytype sialon and phases other than these and measure the respective areas.
- the total amount can be obtained by calculating the ratio of the area of ⁇ -sialon and polytype sialon to the area of the entire photograph.
- the sintered sialon of the present invention not only contains ⁇ -sialon and polytype sialon, but also contains specific ⁇ -sialon and polytype sialon in a specific ratio, as will be described below. Since the rare earth element is contained in a specific ratio, it has chipping resistance, VB wear resistance, and boundary wear resistance. That is, when the sialon sintered body of the present invention is used to cut a work material such as a heat-resistant alloy using the sialon sintered body as a cutting insert, the cutting performance of both roughing and intermediate finishing is long. Can be demonstrated over a period of time.
- the VB wear resistance is a characteristic with respect to wear deterioration mainly due to chemical factors
- the boundary wear resistance is a characteristic with respect to wear deterioration mainly due to physical factors.
- ⁇ -sialon is represented by a general formula of Si 6-Z Al Z O Z N 8-Z , and the Z value is 0.4 or more and 1.0 or less, and 0.6 or more and 0.9 or less. Is preferred.
- a sialon sintered body having all of chipping resistance, VB wear resistance, and boundary wear resistance by having a Z value of 0.4 or more and 1.0 or less, preferably 0.6 or more and 0.9 or less. can be provided.
- the Z value increases, that is, as the amount of Al dissolved in ⁇ -sialon increases, the chemical reaction with the work material such as a heat-resistant alloy is less likely to occur. As a result, chemical wear of the sialon sintered body is suppressed and VB wear resistance is improved.
- the Z value exceeds 1.0, the fracture resistance necessary for roughing the heat-resistant alloy cannot be obtained when the sialon sintered body is used as a cutting insert.
- the Z value is less than 0.4, when the sialon sintered body is used as a cutting insert, the reactivity with a work material such as a heat-resistant alloy is increased and the VB wear resistance is inferior. Therefore, if the Z value is less than 0.4, the VB wear resistance necessary for intermediate finishing cannot be obtained.
- the Z value (Z) can be obtained as follows.
- the a-axis lattice constant of ⁇ -sialon inside 1 mm or more from the burned skin of the sialon sintered body is measured by X-ray diffraction analysis, and the measured value a and the a-axis lattice constant of ⁇ -silicon nitride (7.60442 ⁇ ) are obtained. And can be obtained by the following equation (1).
- Z (a-7.604442) /0.0297 (1)
- each polytype sialon calculated from the peak intensity of the polytype sialon to the total I A of the peak intensity of each sialon calculated from the peak intensity of Sialon obtained by X-ray diffraction analysis The ratio [(I p / I A ) ⁇ 100] of the peak intensity total I p is 10% or more and 50% or less, preferably 10% or more and 40% or less, and preferably 10% or more and 30% or less. Is more preferable.
- a sialon sintered body having all of VB wear resistance and boundary wear resistance can be provided.
- the ratio [(I p / I A ) ⁇ 100] is an index of the content ratio of polytype sialon in the sialon sintered body.
- the ratio [(I p / I A ) ⁇ 100] is less than 10%, the content of polytype sialon in the sialon sintered body is small, so that the effect of improving the VB wear resistance of polytype sialon is improved. Not enough.
- the sialon sintered body has poor VB wear resistance.
- the ratio [(I p / I A ) ⁇ 100] exceeds 50%, the content ratio of polytype sialon in the sialon sintered body is large, and the content ratio of ⁇ -sialon is relatively small. Therefore, it is difficult to form a complex entangled structure of acicular crystal grains, and the sialon sintered body has poor fracture resistance.
- the ratio [(I p / I A ) ⁇ 100] can be obtained as follows. First, X-ray diffraction analysis (XRD) is performed on a sample of a sialon sintered body. As the peak intensity of each sialon obtained by X-ray diffraction analysis, the peak height at the following 2 ⁇ value is used. The following sialons excluding 21R-sialon use the maximum peak in the JCPDS card as peak intensity, whereas 21R-sialon uses peaks other than the maximum peak in the JCPDS card as peak intensity.
- XRD X-ray diffraction analysis
- a value obtained by multiplying the peak intensity obtained by the X-ray diffraction analysis by 2.5 is set as a peak intensity I 21R used for calculation so that it can be compared with the peak height of other sialon.
- the X-ray diffraction chart is compared with the JCPDS card, and a peak that is not easily affected by peaks derived from other sialon is selected.
- the peak intensity I x is multiplied by an appropriate numerical value.
- the sialon sintered body of the present invention is selected from the group consisting of at least one rare earth element B selected from the group consisting of La and Ce, and Y, Nd, Sm, Eu, Gd, Dy, Er, Yb, and Lu. And at least one rare earth element C.
- the sialon sintered body contains the rare earth element B and the rare earth element C
- the raw material powder of the sialon sintered body usually contains the rare earth element B and the rare earth element C.
- a sialon sintered body is produced under the condition that the raw material powder of the sialon sintered body contains only rare earth element C and a Z value of 0.4 to 1.0 is generated, ⁇ -sialon is produced. It is easy to generate.
- the sialon sintered body preferably contains La in the rare earth element B. La is easier to form ⁇ -sialon than Ce and to form a structure in which needle-like crystal grains are intertwined in a complicated manner.
- the sialon sintered body preferably contains at least one selected from the group consisting of Y, Dy, and Er among the rare earth elements C. These rare earth elements C can improve sinterability by adding a small amount.
- the molar ratio M C / M B of the rare earth element B and rare earth elements C is 0.06 to 3.5, preferably 0.1 to 3.0.
- the molar ratio M B : M C is 1.0: 0.06 to 1.0: 3.5, preferably 1.0: 0.1 to 1.0: 3.0 in terms of oxide.
- sialon sintered body having ⁇ -sialon and polytype sialon as the main phases cannot be obtained, resulting in poor VB wear resistance.
- polytype sialon when the molar ratio M C / M B exceeds 3.5, the crystal is liable to precipitate having a garnet-type crystal structure in the grain boundary phase. Therefore, the formed sialon sintered body tends to be brittle, and when used as a cutting insert, it is inferior in fracture resistance and boundary wear resistance, and its life is reduced.
- the total content of rare earth element B and rare earth element C in the sialon sintered body is 0.8 mol% or more and 4.0 mol% or less in terms of oxide, and 1.0 mol% or more and 3.0 mol% or less. Is preferred.
- the content is 0.8 mol% or more and 4.0 mol% or less, preferably 1.0 mol% or more and 3.0 mol% or less, in terms of oxide, ⁇ -sialon and poly Type sialon is easily produced in a desired content ratio. As a result, it is possible to provide a dense sialon sintered body having excellent fracture resistance, VB wear resistance, and boundary wear resistance.
- the sinterability is lowered and it is difficult to obtain a dense sialon sintered body. Even if sintered, the form of ⁇ -sialon does not easily become needle-like, and it is difficult to obtain a structure in which needle-like crystal grains are intertwined in a complicated manner. Therefore, the formed sialon sintered body is inferior in fracture resistance.
- the content is larger than 4.0 mol% in terms of oxide, the grain boundary phase is easily segregated, and as a result, the strength of the sialon sintered body is lowered.
- the formed sialon sintered body is inferior in boundary wear resistance.
- the solid solution rate of Al in ⁇ -sialon is preferably 30% or more and 60% or less. If the solid solution rate of Al in ⁇ -sialon is 30% or more and 60% or less, the balance between the solid solution rate of Al in ⁇ -sialon and the solid solution rate of Al in polytype sialon and grain boundary phase Is good. That is, when the solid solution ratio of Al in ⁇ -sialon is less than 30%, the amount of the grain boundary phase increases and the Al concentration of the grain boundary phase increases. As a result, heat resistance may be reduced.
- the solid solution ratio of Al in ⁇ -sialon is less than 30%, crystals having a garnet-type crystal structure are likely to be precipitated in the grain boundary phase, which makes the sialon sintered body brittle, and has fracture resistance and Boundary wear resistance may be reduced.
- the solid solution ratio of Al is larger than 60%, the amount of the grain boundary phase is reduced, and the Al concentration of the grain boundary phase is lowered. As a result, degranulation is likely to occur, and the VB wear resistance and boundary wear resistance of the sialon sintered body may be reduced.
- the solid solution ratio of Al to ⁇ -sialon is the Z value calculated from the composition of the sialon sintered body assuming that the same amount of Al as that contained in the sialon sintered body is contained in the ⁇ -sialon.
- the theoretical Z value is used, it is represented by the ratio of the Z value to the theoretical Z value [(Z value / theoretical Z value) ⁇ 100].
- the ratio [(Z value / theoretical Z value) ⁇ 100] can be obtained as follows.
- the Z value (Z) is obtained by the X-ray diffraction analysis of the sialon sintered body and the equation (1).
- the theoretical Z value (TZ) is obtained by measuring the content (mass%) of Si and Al contained in the sialon sintered body by fluorescent X-ray analysis or chemical analysis, and measuring the measured Si content as the atomic weight of Si.
- the value obtained by dividing the value by MSi and the value obtained by dividing the measured Al content by the atomic weight of Al is determined by the following formula (2).
- TZ 6MAl / (MSi + MAl) (2)
- the ratio [(Z value / theoretical Z value) ⁇ 100] is calculated from the obtained Z value and the theoretical Z value.
- the sialon sintered body of the present invention preferably does not contain ⁇ -sialon.
- ⁇ -sialon usually has a spherical shape. Therefore, when the sialon sintered body contains ⁇ -sialon, it becomes brittle and the fracture resistance and boundary wear resistance are lowered. On the other hand, when the sialon sintered body contains ⁇ -sialon, the hardness is increased, so that the VB wear resistance is improved. In the case where the sialon sintered body is used as a cutting insert only for the intermediate finishing process, it is preferable to improve the VB wear resistance. Therefore, the sialon sintered body preferably contains ⁇ -sialon.
- the sialon sintered body when used as a cutting insert for general purposes from roughing to semi-finishing, it is necessary to have excellent fracture resistance, VB wear resistance, and boundary wear resistance.
- the sialon sintered body preferably has a low ⁇ -sialon content, and more preferably does not contain it.
- the sialon sintered body of the present invention contains ⁇ -sialon
- fracture resistance VB wear resistance
- a sialon sintered body having boundary wear resistance can be provided.
- M represents the rare earth element B and the rare earth element C.
- the ratio of the atomic ratio a alpha of the rare earth element B with respect to the rare earth element C in sialon sintered body against the rare earth element C in ⁇ - sialon against atomic ratio a S of the rare earth element B a alpha / AS is 70% or less.
- the ⁇ -sialon content in the sialon sintered body is preferably small.
- the sialon sintered body containing ⁇ -sialon that satisfies the condition (1) has a defect resistance, a VB wear resistance, and a boundary wear resistance. All performance can be maintained. It is known that rare earth element B has a large ionic radius and does not penetrate into ⁇ -sialon and dissolve in a single substance.
- the rare earth element B and the rare earth element C are added to the raw material powder of the sialon sintered body, there are some sites where the rare earth element can enter when the rare earth element C enters the ⁇ -sialon and dissolves. Since it spreads, the rare earth element B can enter and dissolve in ⁇ -sialon.
- the ⁇ -sialon in which both the rare earth element B and the rare earth element C are penetrating and forming a solid solution is less likely to cause grain separation than the ⁇ -sialon in which the rare earth element C is penetrating and forming a solid solution alone. Therefore, ⁇ -sialon in which both rare earth element B and rare earth element C enter and dissolves is excellent in boundary wear resistance.
- the ratio A ⁇ / AS is 70% or less, that is, the atomic ratio of the rare earth element B to the rare earth element C is less in the ⁇ -sialon than in the entire sialon sintered body, and is 70% or less.
- the penetration solid solution ratio of the rare earth element B into the glass is small, the interface bonding force between the grain boundary phase and ⁇ -sialon is further increased. As a result, degranulation is less likely to occur, and therefore the boundary wear resistance and fracture resistance are excellent.
- a powder containing an element constituting sialon such as ⁇ -Si 3 N 4 powder, Al 2 O 3 powder, AlN powder, and the like, at least of La 2 O 3 powder and CeO 2 powder which are oxide powders of rare earth element
- At least one of O 3 powder, Yb 2 O 3 powder, and Lu 2 O 3 powder is mixed to obtain a raw material powder.
- 21R-sialon powder may be used instead of AlN.
- a hydroxide may be used instead of the oxide.
- a powder having an average particle size of 5 ⁇ m or less, preferably 3 ⁇ m or less, more preferably 1 ⁇ m or less is preferably used. These raw material powders may be blended in proportion to the composition of the sintered sialon sintered body.
- a raw material powder prepared, an organic binder and ethanol micro wax dissolved in ethanol was added to Si 3 N 4 made pot, with a Si 3 N 4 balls made of raw material powder to wet Mix.
- the obtained slurry is sufficiently dried and press-molded into a desired shape.
- the obtained molded body is degreased for 60 to 120 minutes at 400 to 800 ° C. in a nitrogen atmosphere of 1 atm in a heating apparatus.
- a sialon sintered body can be obtained by placing the degreased compact in a container made of Si 3 N 4 and heating it at 1700-1900 ° C. for 120-360 minutes in a nitrogen atmosphere.
- the theoretical density of the obtained sialon sintered body is less than 99%, it is further subjected to HIP treatment at 1500 to 1700 ° C. for 120 to 240 minutes in a nitrogen atmosphere of 1000 atm, and a dense body having a theoretical density of 99% or more.
- FIG. 1 is a schematic explanatory view showing an embodiment of the cutting insert of the present invention.
- FIG. 2 is a schematic explanatory view showing an embodiment of a cutting tool provided with the cutting insert shown in FIG.
- the cutting insert 1 of this embodiment has a substantially cylindrical shape and is used by being attached to a cutting tool 10.
- the cutting tool 10 is used for cutting heat-resistant alloys and the like, and includes a mounting portion 12 at the distal end portion of the main body portion 11.
- the cutting insert 1 is detachably attached to the attachment portion 12.
- the cutting insert 1 of this embodiment is formed of the sialon sintered body of the present invention. Since this cutting insert 1 is formed of the sialon sintered body described above, it has fracture resistance, VB wear resistance, and boundary wear resistance. In other words, the cutting insert 1 has a chipping resistance that can withstand rough machining of a heat-resistant alloy, a VB wear resistance that is required to obtain a beautiful machined surface by a mid-finishing process, a cutting process of a work material such as Waspaloy, and the like. It has boundary wear resistance that suppresses tooth-like wear that tends to occur at work-hardened locations, and can be used universally from roughing to semi-finishing.
- This cutting insert 1 is suitably used for cutting using a heat-resistant alloy containing Ni as a main component, such as Inconel 718, and a heat-resistant alloy containing Ni as a main component, such as Waspaloy, and containing 10% by mass or more of Co. It is done.
- a heat-resistant alloy containing Ni as a main component such as Inconel 718
- a heat-resistant alloy containing Ni as a main component such as Waspaloy
- the cutting insert of the present invention includes TiN, Ti (C, N), TiC, Al 2 provided on the sialon sintered body and at least a part of the outer peripheral surface of the sialon sintered body.
- O 3 Ti, Al) N, and (Ti, Si) may be formed by a coating film made of various hard carbon nitride represented by N.
- the coating has low reactivity with the work material and high hardness, so the wear resistance is further improved. To do.
- the sialon sintered body of the present invention is not limited to cutting inserts, and can be used as other cutting tools, machine parts, heat resistant parts, wear resistant parts, and the like.
- the degreased compact was placed in a Si 3 N 4 container and heated at 1850 ° C. for 240 minutes in a nitrogen atmosphere to obtain a sialon sintered body.
- the theoretical density of the obtained sialon sintered body was less than 99%, it was further subjected to HIP treatment at 1600 ° C. for 180 minutes in a nitrogen atmosphere of 1000 atm to obtain a dense body having a theoretical density of 99% or more.
- HIP treatment 1600 ° C. for 180 minutes in a nitrogen atmosphere of 1000 atm to obtain a dense body having a theoretical density of 99% or more.
- Table 2 shows the results of analyzing the obtained sialon sintered body.
- the type of sialon contained in the sialon sintered body was identified by X-ray diffraction analysis of the obtained sialon sintered body.
- an amorphous grain boundary phase partially containing crystals was observed between the crystal grains in any of the sialon sintered bodies.
- the Z value of ⁇ -sialon was determined by X-ray diffraction analysis of the obtained sialon sintered body and using equation (1) as described above.
- the solid solution ratio of Al in ⁇ -sialon was determined by subjecting the obtained sialon sintered body to fluorescent X-ray analysis, obtaining the theoretical Z value using equation (2) as described above, and the obtained Z value and The theoretical Z value was determined by substituting it into Z value / theoretical Z value ⁇ 100.
- the content of polytype sialon is obtained a sialon sintered body X-ray diffraction analysis, the proportion of total I p of the peak intensity of each polytype sialon to the total I A of the peak intensity of each sialon as described above [ (I p / I A ) ⁇ 100] was calculated.
- the content of alpha-sialon similarly to the content of polytype sialon, a percentage of the total I A alpha-sialon peak intensity I alpha for the peak intensity of each sialon [(I ⁇ / I A) ⁇ 100] was calculated.
- the contents of rare earth element B and rare earth element C contained in the obtained sialon sintered body were determined by fluorescent X-ray analysis.
- the contents of rare earth element B and rare earth element C contained in ⁇ -sialon are obtained by conducting an EDS analysis of five or more ⁇ -sialon particles using a transmission electron microscope and calculating the average value of the obtained values. It was.
- the cutting insert within the scope of the present invention has a long working distance until reaching any of VB wear, lateral flank boundary wear, chipping, and flaking in cutting, and is resistant to VB. It can be seen that it has wear resistance, boundary wear resistance, and fracture resistance. Therefore, the cutting insert within the scope of the present invention can be used for both roughing and semi-finishing using heat-resistant alloys such as Inconel 718 and Waspaloy as work materials.
- a cutting insert outside the scope of the present invention has a shorter working distance than the cutting insert of the present invention by reaching any one of VB wear, lateral flank boundary wear, chipping, and flaking during cutting. It can be seen that it is inferior to at least one of VB wear resistance, boundary wear resistance, and fracture resistance.
- the cutting insert of test number 25 with a ⁇ -sialon Z value of less than 0.4 has a shorter working distance than cutting inserts within the scope of the present invention.
- the cutting insert of test number 25 has a life factor of VB wear, and it can be seen that when the Z value of ⁇ -sialon is less than 0.4, the VB wear resistance tends to be inferior.
- the cutting inserts with test numbers 20 and 21 having a ⁇ -sialon Z value greater than 1.0 have a shorter working distance than cutting inserts within the scope of the present invention. Moreover, the cutting inserts of test numbers 20 and 21 both include flaking as a life factor. Therefore, it can be seen that if the Z value of ⁇ -sialon is greater than 1.0, flaking is likely to occur and the chipping resistance tends to be inferior.
- the cutting inserts with test numbers 20, 22, 25, and 28 having a polytype sialon content of less than 10% have a shorter working distance than cutting inserts within the scope of the present invention. Since the cutting inserts with test numbers 20 to 22, 25, and 26 do not contain rare earth element B, polytype sialon is hardly generated. Further, the cutting inserts of Test Nos. 22 and 25 containing no polytype sialon have a life factor of VB wear. Therefore, when the polytype sialon content is less than 10%, VB wear resistance tends to be inferior. You can see that
- the cutting inserts with test numbers 18 and 19 having a polytype sialon content of more than 50% have a shorter working distance than cutting inserts within the scope of the present invention.
- the cutting inserts of Test Nos. 18 and 19 often have defects in the lifespan. Therefore, it can be seen that if the content of polytype sialon is larger than 50%, the chipping resistance tends to be inferior.
- the cutting insert of Test No. 24 in which the total content of rare earth element B and rare earth element C is less than 0.8 mol% is inferior in sinterability, and a dense sialon sintered body cannot be obtained. I understand.
- the cutting insert with the test number 23 in which the total content of the rare earth element B and the rare earth element C is greater than 4.0 mol% has a shorter processing distance than the cutting insert within the scope of the present invention.
- the cutting insert of test No. 23 has a life factor of lateral flank boundary wear, and therefore the content of rare earth elements B and C tends to be inferior in boundary wear resistance when the content of the rare earth elements B and C is larger than 4.0 mol%. I understand.
- the cutting insert of Test No. 27 the molar ratio M C / M B is less than 0.06, as compared to the cutting insert within the scope of the present invention, the machining distance short. Further, the cutting insert of Test No. 27, since the include flaking life factors, the molar ratio M C / M B is seen that there is a tendency that poor chipping resistance is less than 0.06.
- the cutting insert molar ratio M C / M B is greater than 3.5 Test No. 28, in comparison with the cutting insert within the scope of the present invention, a short working distance . It can be seen that the cutting insert of test number 28 tends to be inferior in resistance to boundary wear because the life factor is side flank boundary wear. Since the cutting insert of test number 28 contains rare earth element B, ⁇ -sialon can be easily needled, compared to cutting inserts of test numbers 20-22, 25, and 26 that do not contain rare earth element B. It is considered that the fracture resistance is improved.
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Abstract
Description
[1] β-サイアロンと、12H-サイアロン、15R-サイアロン、及び21R-サイアロンからなる群より選択される少なくとも一種のポリタイプサイアロンとを含むサイアロン焼結体であって、
Si6-ZAlZOZN8-Zで表されるβ-サイアロンのZ値が0.4以上1.0以下であり、
X線回折分析により得られるサイアロンのピーク強度から算出される各サイアロンのピーク強度の合計IAに対する前記ポリタイプサイアロンのピーク強度から算出される各ポリタイプサイアロンのピーク強度の合計Ipの割合[(Ip/IA)×100]が10%以上50%以下であり、
La及びCeからなる群より選択される少なくとも一種の希土類元素Bと、Y、Nd、Sm、Eu、Gd、Dy、Er、Yb、及びLuからなる群より選択される少なくとも一種の希土類元素Cとを含み、
前記希土類元素Bと前記希土類元素Cとのモル比MB:MCは、酸化物換算で1.0:0.06~1.0:3.5であり、
前記サイアロン焼結体中における前記希土類元素B及び前記希土類元素Cの合計含有量は、酸化物換算で0.8モル%以上4.0モル%以下であることを特徴とするサイアロン焼結体である。
[2] サイアロン焼結体に含まれるAlと同量のAlがβ-サイアロンに含まれていると仮定してサイアロン焼結体の組成から算出したZ値を理論Z値としたときに、前記理論Z値に対する前記Z値の割合[(Z値/理論Z値)×100]で表されるAlのβ-サイアロンへの固溶率が30%以上60%以下であることを特徴とする[1]に記載のサイアロン焼結体である。
[3] α-サイアロンを含まないことを特徴とする[1]又は[2]に記載のサイアロン焼結体である。
[4] X線回折分析により得られる各サイアロンの前記ピーク強度の合計IAに対するα-サイアロンのピーク強度Iαの割合[(Iα/IA)×100]が10%未満であり、
Mx(Si,Al)12(O,N)16(0<x≦2)で表されるα-サイアロンにおいて、Mは前記希土類元素Bと前記希土類元素Cとを含む金属元素であり、
サイアロン焼結体における希土類元素Cに対する希土類元素Bの原子比ASに対するα-サイアロンにおける希土類元素Cに対する希土類元素Bの原子比Aαの割合Aα/ASが70%以下であることを特徴とする[1]又は[2]に記載のサイアロン焼結体である。
Z=(a-7.60442)/0.0297 ・・・(1)
α-サイアロンのピーク強度Iα:2θ=30.8°付近におけるピーク高さ(α-サイアロンの(2,0,1)面のピーク高さ)
12H-サイアロン(一般式:SiAl5O2N5)のピーク強度I12H:2θ=32.8°付近におけるピーク高さ(12H-サイアロンの(0,0,12)面のピーク高さ)
15R-サイアロン(一般式:SiAl4O2N4)のピーク強度I15R:2θ=32.0°付近におけるピーク高さ(15R-サイアロンの(0,0,15)面のピーク高さ)
21R-サイアロン(一般式:SiAl6O2N6)のピーク強度I21R:2θ=37.6°付近におけるピーク高さ×2.5(21R-サイアロンの(1,0,10)面のピーク高さ×2.5)
TZ=6MAl/(MSi+MAl) ・・・(2)
得られたZ値と理論Z値から前記割合[(Z値/理論Z値)×100]を算出する。
(1)サイアロン焼結体をX線回折分析したときに得られる各サイアロンの前記ピーク強度の合計IAに対するα-サイアロンのピーク強度Iαの割合[(Iα/IA)×100]が10%未満であること
(2)Mx(Si,Al)12(O,N)16(0<x≦2)で表されるα-サイアロンにおいて、Mは前記希土類元素Bと前記希土類元素Cとを含む金属元素であること
(3)サイアロン焼結体における希土類元素Cに対する希土類元素Bの原子比ASに対するα-サイアロンにおける希土類元素Cに対する希土類元素Bの原子比Aαの割合Aα/ASが70%以下であること
である。
平均粒径1.0μm以下のα-Si3N4粉末、Al2O3粉末、AlN粉末と、希土類元素の酸化物粉末とを表1に示す組成となるように配合し、原料粉末とした。次に、配合した原料粉末と、エタノールに溶解したマイクロワックス系の有機バインダとエタノールとを、Si3N4製のポットに投入し、Si3N4製のボールを用いて、原料粉末を湿式混合した。得られたスラリーを十分に乾燥させ、ISO規格でRNGN120700T01020の切削インサートの形状にプレス成形した。得られた成形体を加熱装置内において、1気圧の窒素雰囲気下、約600℃にて、60分間の脱脂処理を施した。さらに、脱脂した成形体をSi3N4製の容器内に配置し、窒素雰囲気下、1850℃で240分間にわたり加熱し、サイアロン焼結体を得た。得られたサイアロン焼結体の理論密度が99%未満の場合は、さらに1000気圧の窒素雰囲気下、1600℃で180分間のHIP処理を行い、理論密度で99%以上の緻密体を得た。このサイアロン焼結体をダイヤモンド砥石で研磨加工することにより、ISO規格でRNGN120700T01020の形状に整え、切削工具用の切削インサートを得た。
表2に得られたサイアロン焼結体を分析した結果を示す。
サイアロン焼結体に含有されるサイアロンの種類は、得られたサイアロン焼結体をX線回折分析することにより同定した。
サイアロン焼結体を走査型電子顕微鏡により観察したところ、いずれのサイアロン焼結体においても結晶粒同士の間に部分的に結晶を含む非晶質の粒界相が観察された。
β-サイアロンのZ値は、得られたサイアロン焼結体をX線回折分析し、前述したように式(1)を用いて求めた。
Alのβ-サイアロンへの固溶率は、得られたサイアロン焼結体を蛍光X線分析して、前述したように式(2)を用いて理論Z値を求め、得られたZ値と理論Z値とを Z値/理論Z値×100 に代入して求めた。
ポリタイプサイアロンの含有量は、得られたサイアロン焼結体をX線回折分析し、前述したように各サイアロンのピーク強度の合計IAに対する各ポリタイプサイアロンのピーク強度の合計Ipの割合[(Ip/IA)×100]を算出して求めた。
α-サイアロンの含有量は、ポリタイプサイアロンの含有量と同様にして、各サイアロンのピーク強度の合計IAに対するα-サイアロンのピーク強度Iαの割合[(Iα/IA)×100]を算出して求めた。
得られたサイアロン焼結体に含まれる、希土類元素B及び希土類元素Cの含有量は、蛍光X線分析により求めた。
α-サイアロンに含まれる希土類元素B及び希土類元素Cの含有量は、透過型電子顕微鏡を用い、5個以上のα-サイアロン粒子をEDS分析し、得られた値の平均値を算出して求めた。
得られた切削インサートを用いて、以下の切削加工条件で切削加工を行った。切削加工において、次のいずれかに達したときの加工距離を表2に示した。なお、欠損とフレーキングとは、切削インサートに現れる損傷の現象としては異なるが、切削インサートの強度及び靱性等同様の特性によって生じる現象である。
(1)VB摩耗(VB)が0.5mmを超えたとき
(2)横逃げ面境界摩耗(VN)が1.0mmを超えたとき
(3)欠損(B)が生じたとき
(4)フレーキング(F)が生じたとき
被削材:インコネル718
切削速度:250m/min
送り速度:0.2mm/rev
切り込み:1.2mm
切削油:あり
被削材:ワスパロイ
切削速度:200m/min
送り速度:0.2mm/rev
切り込み:0.8mm
切削油:あり
β-サイアロンのZ値が0.4未満である試験番号25の切削インサートは、本発明の範囲内にある切削インサートに比べて、加工距離が短い。また、試験番号25の切削インサートは、寿命要因がVB摩耗であることから、β-サイアロンのZ値が0.4未満であると、耐VB摩耗性に劣る傾向にあることが分る。
10 切削工具
11 本体部
12 取付部
Claims (5)
- β-サイアロンと、12H-サイアロン、15R-サイアロン、及び21R-サイアロンからなる群より選択される少なくとも一種のポリタイプサイアロンとを含むサイアロン焼結体であって、
Si6-ZAlZOZN8-Zで表されるβ-サイアロンのZ値が0.4以上1.0以下であり、
X線回折分析により得られるサイアロンのピーク強度から算出される各サイアロンのピーク強度の合計IAに対する前記ポリタイプサイアロンのピーク強度から算出される各ポリタイプサイアロンのピーク強度の合計Ipの割合[(Ip/IA)×100]が10%以上50%以下であり、
La及びCeからなる群より選択される少なくとも一種の希土類元素Bと、Y、Nd、Sm、Eu、Gd、Dy、Er、Yb、及びLuからなる群より選択される少なくとも一種の希土類元素Cとを含み、
前記希土類元素Bと前記希土類元素Cとのモル比MB:MCは、酸化物換算で1.0:0.06~1.0:3.5であり、
前記サイアロン焼結体中における前記希土類元素B及び前記希土類元素Cの合計含有量は、酸化物換算で0.8モル%以上4.0モル%以下であることを特徴とするサイアロン焼結体。 - サイアロン焼結体に含まれるAlと同量のAlがβ-サイアロンに含まれていると仮定してサイアロン焼結体の組成から算出したZ値を理論Z値としたときに、前記理論Z値に対する前記Z値の割合[(Z値/理論Z値)×100]で表されるAlのβ-サイアロンへの固溶率が30%以上60%以下であることを特徴とする請求項1に記載のサイアロン焼結体。
- α-サイアロンを含まないことを特徴とする請求項1又は2に記載のサイアロン焼結体。
- X線回折分析により得られる各サイアロンの前記ピーク強度の合計IAに対するα-サイアロンのピーク強度Iαの割合[(Iα/IA)×100]が10%未満であり、
Mx(Si,Al)12(O,N)16(0<x≦2)で表されるα-サイアロンにおいて、Mは前記希土類元素Bと前記希土類元素Cとを含む金属元素であり、
サイアロン焼結体における希土類元素Cに対する希土類元素Bの原子比ASに対するα-サイアロンにおける希土類元素Cに対する希土類元素Bの原子比Aαの割合Aα/ASが70%以下であることを特徴とする請求項1又は2に記載のサイアロン焼結体。 - 請求項1~4のいずれか一項に記載のサイアロン焼結体からなる切削インサート。
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JP2014513604A JP5629843B1 (ja) | 2013-12-27 | 2013-12-27 | サイアロン焼結体及び切削インサート |
ES13879251T ES2773129T3 (es) | 2013-12-27 | 2013-12-27 | Objeto de sialón sinterizado e inserto de corte |
PCT/JP2013/085085 WO2015097856A1 (ja) | 2013-12-27 | 2013-12-27 | サイアロン焼結体及び切削インサート |
US14/389,436 US9695087B2 (en) | 2013-12-27 | 2013-12-27 | Sialon sintered body and cutting insert |
KR1020147027635A KR101609090B1 (ko) | 2013-12-27 | 2013-12-27 | 사이알론 소결체 및 절삭 인서트 |
EP13879251.0A EP3088375B1 (en) | 2013-12-27 | 2013-12-27 | Sintered sialon object and cutting insert |
MX2016005467A MX2016005467A (es) | 2013-12-27 | 2013-12-27 | Cuerpo sinterizado de sialon e inserto de corte. |
CA2868293A CA2868293C (en) | 2013-12-27 | 2013-12-27 | Sialon sintered body and cutting insert |
CN201380018267.7A CN104884410B (zh) | 2013-12-27 | 2013-12-27 | 赛隆烧结体和切削刀片 |
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WO2016052468A1 (ja) * | 2014-09-29 | 2016-04-07 | 日本特殊陶業株式会社 | サイアロン焼結体及び切削インサート |
JP2019077576A (ja) * | 2017-10-23 | 2019-05-23 | 島根県 | サイアロン材料の耐高温反応性改善方法、該方法を用いたサイアロン材料の製造方法、及びサイアロンセラミックス工具 |
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KR102328799B1 (ko) * | 2014-11-13 | 2021-11-18 | 대구텍 유한책임회사 | 세라믹 재료 및 이 세라믹 재료로 만들어진 절삭 공구 |
JP7340622B2 (ja) * | 2019-12-20 | 2023-09-07 | Ntkカッティングツールズ株式会社 | 切削工具 |
RU2757607C1 (ru) * | 2021-04-12 | 2021-10-19 | Федеральное государственное бюджетное учреждение науки Институт металлургии и материаловедения им. А.А. Байкова Российской академии наук (ИМЕТ РАН) | Способ получения 21R-сиалоновой керамики |
EP4249451A1 (de) * | 2022-03-21 | 2023-09-27 | CeramTec GmbH | Keramischer sinterformkörper aus einem sialon-werkstoff, seine rohstoffmischung und herstellung |
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