WO2016171155A1 - 焼結体およびそれを含む切削工具 - Google Patents
焼結体およびそれを含む切削工具 Download PDFInfo
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- WO2016171155A1 WO2016171155A1 PCT/JP2016/062460 JP2016062460W WO2016171155A1 WO 2016171155 A1 WO2016171155 A1 WO 2016171155A1 JP 2016062460 W JP2016062460 W JP 2016062460W WO 2016171155 A1 WO2016171155 A1 WO 2016171155A1
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- WIPO (PCT)
- Prior art keywords
- sintered body
- volume
- phase
- zro
- particle size
- Prior art date
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- 238000005520 cutting process Methods 0.000 title claims description 54
- 239000000463 material Substances 0.000 claims abstract description 134
- 239000013078 crystal Substances 0.000 claims abstract description 40
- 229910052582 BN Inorganic materials 0.000 claims abstract description 23
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 116
- 239000002245 particle Substances 0.000 claims description 80
- 150000001875 compounds Chemical class 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 4
- 239000000395 magnesium oxide Substances 0.000 claims description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 4
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052796 boron Inorganic materials 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 3
- 229910021480 group 4 element Inorganic materials 0.000 claims description 3
- 229910021478 group 5 element Inorganic materials 0.000 claims description 3
- 229910021476 group 6 element Inorganic materials 0.000 claims description 3
- 229910000449 hafnium oxide Inorganic materials 0.000 claims description 3
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 3
- 230000000737 periodic effect Effects 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract description 18
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 38
- 238000000034 method Methods 0.000 description 30
- 238000005245 sintering Methods 0.000 description 23
- 239000000203 mixture Substances 0.000 description 10
- 239000002243 precursor Substances 0.000 description 10
- 239000006104 solid solution Substances 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 238000002156 mixing Methods 0.000 description 9
- 239000002994 raw material Substances 0.000 description 8
- 238000006386 neutralization reaction Methods 0.000 description 7
- 238000012545 processing Methods 0.000 description 7
- 238000000682 scanning probe acoustic microscopy Methods 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 238000000921 elemental analysis Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000005299 abrasion Methods 0.000 description 5
- 238000000975 co-precipitation Methods 0.000 description 5
- 238000010884 ion-beam technique Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000007921 spray Substances 0.000 description 5
- 229910001018 Cast iron Inorganic materials 0.000 description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 4
- 238000005469 granulation Methods 0.000 description 4
- 230000003179 granulation Effects 0.000 description 4
- 239000011268 mixed slurry Substances 0.000 description 4
- 238000004663 powder metallurgy Methods 0.000 description 4
- 238000003980 solgel method Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 150000003746 yttrium Chemical class 0.000 description 3
- 150000003754 zirconium Chemical class 0.000 description 3
- 229910052726 zirconium Inorganic materials 0.000 description 3
- OBOSXEWFRARQPU-UHFFFAOYSA-N 2-n,2-n-dimethylpyridine-2,5-diamine Chemical compound CN(C)C1=CC=C(N)C=N1 OBOSXEWFRARQPU-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- -1 etc.) Inorganic materials 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000010191 image analysis Methods 0.000 description 2
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- KJPRLNWUNMBNBZ-QPJJXVBHSA-N (E)-cinnamaldehyde Chemical compound O=C\C=C\C1=CC=CC=C1 KJPRLNWUNMBNBZ-QPJJXVBHSA-N 0.000 description 1
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000007909 melt granulation Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- UJVRJBAUJYZFIX-UHFFFAOYSA-N nitric acid;oxozirconium Chemical compound [Zr]=O.O[N+]([O-])=O.O[N+]([O-])=O UJVRJBAUJYZFIX-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910001562 pearlite Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000002490 spark plasma sintering Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/486—Fine ceramics
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- C04B35/4885—Composites with aluminium oxide
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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
- C04B35/583—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 based on boron nitride
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Definitions
- the present invention relates to a sintered body and a cutting tool including the same.
- ZrO 2 —Al 2 O 3 based solid solution ceramics are used in various ceramic parts (International Publication No. 2012/153645 (Patent Document 4), Japanese Patent Application Laid-Open No. 2014-189474 (Patent Document 5)). .
- the present invention has been made in view of such circumstances, and an object of the present invention is to provide a sintered body having improved wear resistance and high wear resistance in high-speed cutting. .
- the sintered body according to one embodiment of the present invention includes a first material and cubic boron nitride, and the first material contains 5 to 90% by volume of Al 2 O 3 as crystal grain boundaries or crystals. Partially stabilized ZrO 2 dispersed in the grains.
- the fracture resistance in high-speed cutting is improved and the wear resistance is good.
- a sintered body according to one embodiment of the present invention includes a first material and cubic boron nitride, and the first material includes 5 to 90% by volume of Al 2 O 3 crystal grains. Partially stabilized ZrO 2 dispersed in the boundaries or crystal grains. This sintered body has improved wear resistance in high speed cutting and has good wear resistance.
- the first material may be partially stabilized ZrO 2 in which 5 to 50% by volume of Al 2 O 3 is dispersed in crystal grain boundaries or crystal grains. Thereby, the fracture resistance in high speed cutting is improved.
- the first material is a partially stabilized ZrO 2 in which Al 2 O 3 of more than 50% by volume and 70% by volume or less (above 50% by volume and 70% by volume or less) is dispersed in the crystal grain boundaries or crystal grains. can do. Thereby, it becomes what was excellent in abrasion resistance especially.
- the first material includes partially stabilized ZrO 2 in which Al 2 O 3 of more than 70% by volume and 90% by volume or less (above 70% by volume and 90% by volume or less) is dispersed in the crystal grain boundaries or crystal grains. can do. Thereby, it becomes what was excellent in abrasion resistance especially.
- the Al 2 O 3 is preferably a particle having a particle size of 1 ⁇ m or less. Thereby, the toughness of partially stabilized ZrO 2 is improved.
- the Al 2 O 3 is more preferably a particle having a particle size of 0.5 ⁇ m or less. Thereby, the toughness of partially stabilized ZrO 2 is further improved.
- the Al 2 O 3 is more preferably a particle having a particle size of 0.1 ⁇ m or less. Thereby, the toughness of partially stabilized ZrO 2 is further improved.
- the sintered body preferably includes 20 to 80% by volume of the first material. As a result, the wear resistance and fracture resistance of the sintered body are more highly compatible.
- the sintered body further includes a third phase, and the third phase is at least one selected from the group consisting of aluminum oxide, magnesium oxide, cerium oxide, yttrium oxide, hafnium oxide, and ZrO. It is preferable. Thereby, sinterability improves and the intensity
- the sintered body further includes a fourth phase, and the fourth phase is at least one selected from the group consisting of Group 4 elements, Group 5 elements, Group 6 elements, Al, and Si in the periodic table. And at least one compound comprising at least one element selected from the group consisting of carbon, nitrogen, and boron. This also improves the sinterability and further improves the strength of the sintered body.
- One aspect of the present invention also relates to a cutting tool including any one of the above sintered bodies. Since this cutting tool includes the above-mentioned sintered body, it has improved fracture resistance in high-speed cutting and has good wear resistance.
- the sintered body of the present embodiment obtained based on such knowledge includes a first material and cubic boron nitride, and the first material is 5 to 90% by volume (5% by volume). 90% by volume or less, and in the present application, when the numerical range is expressed by using “ ⁇ ”, the range includes the upper and lower limit numerical values) Al 2 O 3 dispersed in the crystal grain boundaries or crystal grains Stabilized ZrO 2 .
- Such a sintered body may contain any other component as long as it contains the first material and cubic boron nitride.
- examples of other optional components include, but are not limited to, a third phase and a fourth phase described later.
- such a sintered body can contain inevitable impurities as long as the desired effect is exhibited.
- such a sintered body may include only both the first material and cubic boron nitride.
- the first material is partially stabilized ZrO 2 in which 5 to 90% by volume of Al 2 O 3 is dispersed in the crystal grain boundaries or crystal grains.
- the first material is a complex oxide in which 5 to 90% by volume of Al 2 O 3 is dispersed in the crystal grain boundaries or crystal grains of partially stabilized ZrO 2 .
- the partially stabilized ZrO 2 has a conventionally known meaning.
- an oxide other than zirconia oxygen vacancies in the structure are reduced and stabilized.
- it refers to ZrO 2 in which cubic crystals and tetragonal crystals are stable or metastable at room temperature.
- the oxide include calcium oxide and magnesium oxide, and rare earth oxides such as yttrium oxide. One or more of such oxides can be included.
- the solid solution amount of oxides other than zirconia is about 1 to 4 mol% with respect to ZrO 2 .
- Such partially stabilized ZrO 2 contains 5 to 90% by volume of Al 2 O 3 with respect to the entire first material.
- content of Al 2 O 3 when the content is 5 to 50% by volume with respect to the entire first material, it is possible to cut a steel difficult-to-cut material at high speed. Strength and high toughness can be obtained.
- a more preferable content in this case is 15 to 30% by volume.
- the content of Al 2 O 3 is less than 5% by volume, the above characteristics cannot be obtained.
- the wear resistance is improved. That is, when the content of Al 2 O 3 is within this range, the first material containing not less than Al 2 O 3 alone and 5 to 50% by volume of Al 2 O 3 in high-speed cutting of steel difficult-to-cut materials. More abrasion resistance than that obtained when using is obtained.
- the wear resistance is more preferably improved when the content is in the range of more than 50% by volume and not more than 70% by volume than in the range of more than 70% by volume and not more than 90% by volume. When the content of Al 2 O 3 exceeds 90% by volume, performance exceeding that of Al 2 O 3 alone cannot be obtained.
- Al 2 O 3 is dispersed and present in the crystal grain boundaries or crystal grains of the partially stabilized ZrO 2 . That is, “present in a dispersed state” means that fine Al 2 O 3 exists in the crystal grain boundaries or crystal grains. Therefore, Al 2 O 3 is preferably particles (crystal grains) of 1 ⁇ m or less, more preferably particles of 0.5 ⁇ m or less, and further preferably particles of 0.1 ⁇ m or less. The lower the particle size, the more tend to improve the toughness, so the lower limit of the particle size is not particularly limited, but from the viewpoint of reducing the toughness of the substance itself if too fine, 0.005 ⁇ m or more It is preferable.
- the particle diameter of such Al 2 O 3 has a feature that varies with the sintering conditions. Moreover, even under the same sintering conditions, the particle size of Al 2 O 3 is different between the case where only the first material is sintered and the case where the first material and cubic boron nitride are mixed and sintered. Change.
- the particle size of Al 2 O 3 when only the first material is sintered is compared with the particle size of Al 2 O 3 when the first material and cubic boron nitride are mixed and sintered, Even if the same sintering conditions (temperature, pressure, etc.) are employed, the latter particle size (ie, the particle size of Al 2 O 3 in the sintered body containing cubic boron nitride) is the former particle size (ie, the first particle size).
- the grain size is about 1/10 (crystal grain size).
- the grain size (crystal grain size) of Al 2 O 3 is 0.1 ⁇ m or less is a specific phenomenon that appears when the first material and cubic boron nitride are mixed and sintered, When cubic boron nitride is not included, the particle size of Al 2 O 3 does not become 0.1 ⁇ m or less (usually a particle size exceeding 0.2 ⁇ m).
- Al 2 O 3 is remarkably improved in toughness by being finely dispersed in the first material. This is considered to be due to the strengthening of the structure by Al 2 O 3 .
- Al 2 O 3 can be present at either or both of the crystal grain boundaries and crystal grains. That is, this means that the location of Al 2 O 3 is not limited to a specific location of partially stabilized ZrO 2 .
- the particle diameter, content (volume%) and location of Al 2 O 3 can be confirmed as follows. That is, the sintered body is subjected to CP (Cross Section Polisher) processing using an ion beam to form a smooth cross section. Then, by observing the cross section with a scanning electron microscope (SEM), the location of Al 2 O 3 is specified, and the equivalent circle diameter of Al 2 O 3 is determined by binarization using image analysis software. The area is calculated, and the equivalent circle diameter is the particle diameter and the area is the content.
- CP Cross Section Polisher
- the raw material of the first material of the present embodiment can be obtained, for example, by the following neutralization coprecipitation method or sol-gel method.
- the neutralization coprecipitation method is a method including the following step A and step B. Such a method is described, for example, in a paper published in 2013 (J. Jpn. Soc. Powder Powder Metallurgy, Vol. 60, No. 10, P428-435).
- Step A Using a zirconium salt, an yttrium salt, and an aluminum salt, the molar ratio as zirconia (ZrO 2 ) and yttria (Y 2 O 3 ) is 98.2: 1.8 to 98.8: 1.2, and And yttria-added zirconia and alumina (Al 2 O 3 ) are mixed at a molar ratio of 10:90 to 95: 5 to prepare a mixed solution.
- yttria (Y 2 O 3 ) is exemplified as an oxide solid-dissolved in zirconia (ZrO 2 ), but the oxide is not limited to this.
- Step B Neutralization is performed by adding alkali to the mixed solution obtained in the above step A, and zirconium, yttrium, and aluminum are coprecipitated to obtain a precipitate. After the precipitate is dried, 650 to A step of preparing a Y 2 O 3 stabilized ZrO 2 —Al 2 O 3 solid solution powder by heat treatment at 750 ° C. for 7 to 12 hours and further calcining at 850 to 950 ° C. for 0.5 to 3 hours.
- examples of the zirconium salt in Step A include zirconium oxychloride (ZrOCl 2 ) and zirconium oxynitrate (ZrO (NO 3 ) 2 ).
- examples of the yttrium salt include yttrium chloride (YCl 3 ), Examples thereof include yttrium nitrate (Y (NO 3 ) 3 ), and examples of the aluminum salt include aluminum chloride (AlCl 3 ).
- nitric acid, hydrochloric acid, etc. can be mentioned as a solvent used as a mixed solution.
- the sol-gel method is a method including the following step X. Such a method is described, for example, in a paper published in 2011 (J. Jpn. Soc. Powder Powder Metallurgy, Vol. 58, No. 12, P727-732).
- Step X Sol - to ZrO 2 using a gel method 0.3 ⁇ 1.7mol% Y 2 O 3 ZrO 2 was added (99.7 ⁇ 98.3mol% ZrO 2 -0.3 ⁇ 1.7mol % Y 2 O 3 ) ⁇ 5 to 90 mol% Al 2 O 3 amorphous solid solution powder, and the resulting amorphous solid solution powder is calcined above the crystallization temperature to obtain a crystalline ZrO 2 solid solution.
- a step of preparing a powder Sol - to ZrO 2 using a gel method 0.3 ⁇ 1.7mol% Y 2 O 3 ZrO 2 was added (99.7 ⁇ 98.3mol% ZrO 2 -0.3 ⁇ 1.7mol % Y 2 O 3 ) ⁇ 5 to 90 mol% Al 2 O 3 amorphous solid solution powder, and the resulting amorphous solid solution powder is calcined above the crystallization temperature to obtain a crystalline ZrO 2 solid solution.
- the first material of this embodiment can also be obtained by methods other than the above two methods. That is, partially stabilized ZrO 2 and Al 2 O 3 are mixed in a solvent such as ethanol using a pulverizer such as a bead mill or a ball mill to obtain a slurry. Next, the first material can be obtained by granulation using this slurry.
- the granulating means is not particularly limited, and examples thereof include melt granulation and spray granulation.
- the granulated product (first material) thus obtained can be improved in strength by the following method.
- Sintering is performed in a heat treatment furnace (for example, 1000 ° C. in vacuum for 3 hours).
- a binder for example, PVB (polyvinyl butyral) which is a general binder
- PVB polyvinyl butyral
- the first material can be obtained by various methods, and the manufacturing method is not particularly limited.
- Such a first material is preferably contained in the sintered body in a proportion of 20 to 80% by volume. If the ratio is less than 20% by volume, the wear resistance and fracture resistance may be lowered. Moreover, when the ratio exceeds 80 volume%, hardness may fall and abrasion resistance may fall. A more desirable ratio of the first material is 30% to 60% by volume.
- such a first material preferably has an average particle diameter of 0.01 to 1 ⁇ m. If it is less than 0.01 ⁇ m, it tends to agglomerate when mixed with other powders, which tends to cause poor sintering. If it exceeds 1 ⁇ m, the strength tends to decrease due to grain growth during sintering.
- a more preferable average particle diameter is 0.1 to 0.5 ⁇ m.
- the average particle diameter of the first material can be obtained as follows. That is, the sintered body is processed by CP (Cross Section Polisher) using an ion beam to form a smooth cross section, and the cross section is observed with a scanning electron microscope (SEM).
- the equivalent circle diameter of the first material can be calculated by the valuation process, and can be used as the average particle diameter.
- each component composition which comprises the sintered compact of this embodiment including this 1st material, and its content rate are the backscattered electron image which measured the CP processed surface with the scanning electron microscope (SEM), EDX (energy dispersion
- SEM scanning electron microscope
- EDX energy dispersion
- the cubic boron nitride contained in the sintered body of the present embodiment preferably has an average particle size of 0.1 to 5 ⁇ m. If it is less than 0.1 ⁇ m, it tends to agglomerate when mixed with other powders, which tends to cause poor sintering. If it exceeds 5 ⁇ m, the strength tends to decrease due to grain growth during sintering.
- the particle diameter of such cubic boron nitride is preferably uniform from the viewpoint of high strength without stress concentration, and therefore the average particle diameter herein preferably shows a normal distribution.
- the average particle size shows a normal distribution and is uniform.
- Such cubic boron nitride is preferably contained in the sintered body in a proportion of 20 to 80% by volume. If the ratio is less than 20% by volume, the hardness may decrease and the wear resistance may decrease. On the other hand, if the ratio exceeds 80% by volume, the wear resistance and fracture resistance may decrease. A more desirable ratio of cubic boron nitride is 40 to 60% by volume.
- the average particle diameter of cubic boron nitride can be obtained as follows. That is, the sintered body is processed by CP (Cross Section Polisher) using an ion beam to form a smooth cross section, and the cross section is observed with a scanning electron microscope (SEM). The equivalent circle diameter of cubic boron nitride can be calculated by the valuation process, and can be used as the average particle diameter.
- the content ratio of cubic boron nitride can be obtained by measuring the area by binarization processing using image analysis software of a reflected electron image obtained by measuring the CP processed surface with a scanning electron microscope (SEM).
- the sintered body of the present embodiment can further include a third phase in addition to the first material and cubic boron nitride.
- a third phase is preferably at least one selected from the group consisting of aluminum oxide, magnesium oxide, cerium oxide, yttrium oxide, hafnium oxide, and ZrO.
- Such a third phase preferably has an average particle diameter of 0.05 to 5 ⁇ m. If it is less than 0.05 ⁇ m, it tends to agglomerate when mixed with other powders, so that it tends to cause sintering failure. If it exceeds 5 ⁇ m, the strength tends to decrease due to grain growth during sintering.
- such a third phase is preferably contained in the sintered body at a ratio of 5 to 50% by volume. If the ratio is less than 5% by volume, the strength of the sintered body may not be sufficiently improved. Moreover, when the ratio exceeds 50 volume%, the ratio of high hardness cBN may fall and the hardness of a sintered compact may fall. A more desirable ratio of the third phase is 10 to 30% by volume.
- the average particle size of the third phase can be obtained as follows. That is, the sintered body is processed by CP (Cross Section Polisher) using an ion beam to form a smooth cross section, and the cross section is observed with a scanning electron microscope (SEM).
- the equivalent circle diameter of the third phase is calculated by the valuation process, and can be used as the average particle diameter.
- the content ratio of the third phase is determined by image analysis after confirming the region of the third phase by a reflected electron image obtained by measuring the CP processed surface by a scanning electron microscope (SEM) or by elemental analysis by Auger electron spectroscopy.
- SEM scanning electron microscope
- the area can be measured and obtained by binarization processing using software.
- the sintered body of the present embodiment can further include a fourth phase in addition to the first material and cubic boron nitride.
- the fourth phase may be included in the sintered body together with the third phase.
- Such a fourth phase includes Group 4 elements of the periodic table (Ti, Zr, Hf, etc.), Group 5 elements (V, Nb, Ta, etc.), Group 6 elements (Cr, Mo, W, etc.), Al, and It is preferably at least one compound consisting of at least one element selected from the group consisting of Si and at least one element selected from the group consisting of carbon, nitrogen, and boron.
- the sintered body contains such a fourth phase, the sinterability is improved and the strength of the sintered body is further improved.
- the above compounds include, for example, TiC, TiN, TiB 2 , TiCrN, ZrC, ZrN, ZrB 2 , AlCrN, AlN, AlB 2 , SiC, Si 3 N 4 , HfC, HfN, VC, VN, NbC , TaC, CrC, CrN, Cr 2 N, MoC, WC and the like.
- the fourth phase can be composed of one of these compounds alone or a combination of two or more.
- Such a fourth phase preferably has an average particle diameter of 0.05 to 5 ⁇ m. If it is less than 0.05 ⁇ m, it tends to agglomerate when mixed with other powders, so that it tends to cause sintering failure. If it exceeds 5 ⁇ m, the strength tends to decrease due to grain growth during sintering.
- such a fourth phase is preferably contained in the sintered body at a ratio of 5 to 50% by volume. If the ratio is less than 5% by volume, the strength of the sintered body may not be sufficiently improved. Moreover, when the ratio exceeds 50 volume%, the ratio of high hardness cBN may fall and the hardness of a sintered compact may fall. A more desirable ratio of the fourth phase is 10 to 30% by volume.
- the average particle size of the fourth phase can be obtained as follows. That is, the sintered body is processed by CP (Cross Section Polisher) using an ion beam to form a smooth cross section, and the cross section is observed with a scanning electron microscope (SEM).
- the equivalent circle diameter of the fourth phase can be calculated by the valuation process, and can be used as the average particle diameter.
- the content ratio of the fourth phase is determined by image analysis after confirming the region of the fourth phase by a reflected electron image obtained by measuring the CP processed surface by a scanning electron microscope (SEM) or by elemental analysis by Auger electron spectroscopy.
- SEM scanning electron microscope
- the area can be measured and obtained by binarization processing using software.
- the sintered body of the present embodiment can be manufactured by a conventionally known manufacturing method, and the manufacturing method is not particularly limited.
- the first material, cBN, and other components are mixed in a bead mill, ball mill, or the like. Subsequently, it can be obtained by sintering at a temperature of 1300 to 1700 ° C. and a pressure of 10 MPa to 7 GPa for 10 to 60 minutes, particularly preferably 4 to 7 GPa.
- the sintering method is not particularly limited, spark plasma sintering (SPS), hot press, ultra-high pressure press, or the like can be used.
- the sintered body of the present embodiment exhibits excellent characteristics such as fracture resistance and wear resistance as described above, it is preferable to use it for a cutting tool or the like. That is, the cutting tool of the present embodiment includes the above sintered body.
- the cutting tool includes a drill, an end mill, a cutting edge exchangeable cutting tip for a drill, a cutting edge exchangeable cutting tip for an end mill, a cutting edge exchangeable cutting tip for milling, a cutting edge exchangeable cutting tip for turning, a metal saw, a tooth
- Examples include cutting tools, reamers, taps, cutting tools, and the like.
- the cutting tool may be entirely constituted by the sintered body of the present embodiment, or only a part (for example, a blade edge portion) may be constituted by the sintered body of the present embodiment. good. Moreover, such a cutting tool may have a coating film formed on the surface thereof.
- Example 1 As raw materials, 60% by volume of cBN and 40% by volume of a first material were prepared. cBN has an average particle diameter of 2 ⁇ m, and the first material was prepared by the neutralization coprecipitation method as described below, and 30% by volume of Al 2 O 3 was dissolved in the entire first material. It was partially stabilized ZrO 2 and the particle size was 0.01 ⁇ m.
- the first material can be produced by the following method based on a paper published in 2013 (J. Jpn. Soc. Powder Powder Metallurgy, Vol. 60, No. 10, P428-435).
- the solid solution powder obtained above is calcined (heat treated) at 700 ° C. in air for 9 hours, and further calcined at 900 ° C. for 1 hour to form a first material (precursor).
- a crystalline ZrO 2 (Al 2 O 3 , Y 2 O 3 solid solution) powder is obtained.
- This first material (precursor) is partially stabilized ZrO 2 in which 30% by volume of Al 2 O 3 is dissolved in the entire first material.
- the cBN prepared above and the first material (precursor) were mixed using a ball mill to obtain a mixture.
- the above mixture was divided into five equal parts, sintered at a pressure of 7 GPa and a sintering temperature of 15 minutes while maintaining the sintering temperature for 15 minutes.
- 1 to sintered body No. 1 5 types of sintered bodies were obtained.
- the average particle size of cBN was the same as the average particle size of the raw material, but the Al 2 O 3 particles in the first material It was confirmed that the diameter varied depending on the sintering temperature.
- the sintered body No. 1 to sintered body No. 1 For No. 5 after confirming the region of cBN and the first material by the reflected electron image obtained by measuring the CP processed surface with a scanning electron microscope (SEM) or by elemental analysis by Auger electron spectroscopy, the above image analysis software is used.
- SEM scanning electron microscope
- Auger electron spectroscopy the above image analysis software is used.
- each sintered body contained the first material and cBN, and it was also confirmed that the ratio of the first material and cBN coincided with the raw material ratio.
- the first material is partially stabilized ZrO 2 in which 30% by volume of Al 2 O 3 is dispersed in the crystal grain boundaries or crystal grains.
- the sintered body No. 1 to sintered body No. 1 A cutting tool having a shape of CNMA 120408, a negative land angle of 15 °, and a negative land width of 0.12 mm was produced using each of the sintered bodies of No. 5, and a high-speed cutting test was performed under the following cutting conditions.
- the sintered body No. 6 was produced as follows. That is, 60 vol% cBN (same as above), 34 vol% ZrO 2 (average particle size 0.05 ⁇ m), and 6 vol% Al 2 O 3 (average particle size 2 ⁇ m) were prepared. Each powder of ZrO 2 and Al 2 O 3 replaces the first material, and the ZrO 2 powder does not contain Al 2 O 3 (in Table 1, the average particle size of the Al 2 O 3 powder is the first material for convenience. In the column of average particle diameter in the middle).
- the sintered body No. 1-No. 5 is a sintered body No. 5 of the comparative example. Compared to 6, the flank wear after 10.0 km cutting is small and the wear resistance is excellent, and the wear form after 12.0 km cutting is also good, and it can be confirmed that it has excellent fracture resistance. It was.
- the sintered body No. 1-No. 5 was compared, it was confirmed that the lower the sintering temperature, the smaller the average particle size of Al 2 O 3 , and both the wear resistance and the fracture resistance were more excellent.
- Sintered body No. 7 to sintered body No. Table 1 shows the results of measuring the particle size of Al 2 O 3 and the results of the cutting test for No. 10 in the same manner as described above.
- Example 2 Except for changing the content of the first material in the sintered body as shown in Table 2 below, everything else is the sintered body No. 1 of Example 1. 7 (that is, those having a sintering temperature of 1500 ° C.), seven types of sintered bodies were produced (sintered bodies No. 3a, No. 3b, No. 3c, No. 3d, No. 3e, No. 3f, No. 3g).
- the location of Al 2 O 3 in the first material was specified by the same method as in Example 1, and the equivalent circle diameter (particle size) of Al 2 O 3 and contained When the amount was calculated, the sintered body No. 3 was confirmed to be the same. Further, by the same method as in Example 1, it was confirmed that the composition (content of the first material) of each sintered body was as shown in Table 2.
- Example 3 Except for changing the content of Al 2 O 3 in the first material as shown in Table 3 below, everything else is the sintered body No. 1 of Example 1. In the same manner as in Example 3, seven types of sintered bodies were produced (sintered bodies No. 3t, No. 3u, No. 3v, No. 3w, No. 3x, No. 3y, No. 3z).
- the sintered body No. 3t are those first material is composed of only Al 2 O 3 (ie the content of Al 2 O 3 is made of Al 2 O 3 alone as a 100% by volume), such Al 2 O Daimyo Chemical Co., Ltd. TM-DAR was used as 3 .
- the location of Al 2 O 3 in the first material was specified by the same method as in Example 1, and the equivalent circle diameter (particle size) of Al 2 O 3 and contained
- the sintered body No. 1 of Example 1 was excluded except for the content of Al 2 O 3 . 3 was confirmed to be the same.
- the composition of each sintered body was confirmed by the same method as in Example 1, the sintered body No. 1 in Example 1 was excluded except for the content of Al 2 O 3 . 3 was confirmed to be the same.
- the content of Al 2 O 3 of the first material is intended to adjust the content of Al 2 O 3 at the time of preparation by neutralization co-precipitation as described above.
- the sintered body No. Except for 3t all of the sintered bodies showed excellent wear resistance and fracture resistance.
- Example 4 Except for replacing the first material (content: 40% by volume) in the sintered body with 23% by volume of the first material and 17% by volume of the third phase and / or the fourth phase described in Table 4, Other than the above, the sintered body No. 1 of Example 1 was used. In the same manner as in No. 3, 24 types of sintered bodies were produced (sintered bodies No. 301 to No. 324).
- the location of Al 2 O 3 in the first material is specified by the same method as in Example 1, and the equivalent circle diameter (particle size) and content of Al 2 O 3 are contained.
- the sintered body No. 3 was confirmed to be the same.
- the region of cBN, the first material, the third phase, and the fourth phase is obtained by a reflected electron image obtained by measuring the CP processed surface of each sintered body with a scanning electron microscope (SEM) or by elemental analysis by Auger electron spectroscopy.
- SEM scanning electron microscope
- the area was measured by binarization processing using the above image analysis software, and the composition and content of cBN, the first material, the third phase, and the fourth phase are as described above and in Table 4 It was confirmed that it was the same.
- Example 5 The sintered body of Example 1 except that the first material (content: 40% by volume) in the sintered body is replaced with the following first material (1) to first material (6), respectively. No. In the same manner as in No. 3, six types of sintered bodies were produced.
- First material (1) Partially stabilized ZrO 2 powder (trade name: “TZ-3Y”, manufactured by Tosoh, average particle size: 45 nm) and Al 2 O 3 powder (trade name: “TM-DAR”, manufactured by Daimei Chemical, average particle size: 0) 0.1 ⁇ m) in a solvent (ethanol) using a ball mill to obtain a mixed slurry.
- the mixing ratio of both powders is such that the content ratio in the sintered body is 34 vol% for ZrO 2 and 6 vol% for Al 2 O 3 (ratio in the first material: 15 vol%).
- the mixed slurry obtained above was granulated (spray granulation) with a spray dryer (trade name: “FR125”, manufactured by Pris) to obtain a granulated powder.
- the granulated powder was sintered under a condition of “1000 ° C. in a vacuum for 3 hours” using a heat treatment furnace to obtain a first material (1) which is a granulated product with enhanced strength. .
- First material (2) Partially stabilized ZrO 2 powder and Al 2 O 3 powder are contained in a sintered body in a proportion of 28% by volume of ZrO 2 and 12% by volume of Al 2 O 3 (ratio in the first material: 30 volumes). %) Except that mixing was performed to obtain the first material (2) in the same manner as the first material (1).
- First material (3) The partially stabilized ZrO 2 powder and the Al 2 O 3 powder are 20% by volume of ZrO 2 and 20% by volume of Al 2 O 3 in the sintered body (ratio in the first material: 50 volumes). %) Except that mixing was performed to obtain the first material (3) in the same manner as the first material (1).
- the mixed slurry obtained above was granulated (spray granulation) with a spray dryer (trade name: “FR125”, manufactured by Pris) to obtain a granulated powder, which was used as the first material (4). .
- Example 5 The same cutting test as in Example 1 was performed using the six types of sintered bodies obtained as described above. The results are shown in Table 5 below.
- the location of Al 2 O 3 in the first material is specified by the same method as in Example 1, and the equivalent circle diameter (particle size) of Al 2 O 3 and contained
- the particle size of the first material was approximately 0.15 ⁇ m
- the particle size of Al 2 O 3 was 0.1 ⁇ m
- the content ratio of ZrO 2 and Al 2 O 3 in the sintered body was almost as described above.
- Example 6 Replacing the first material in the sintered body with the first material produced as follows (this first material is referred to as “first material A” for convenience) (that is, the first material precursor of the sintered body raw material) Except for replacing the body with the following “first material A”), everything else is the sintered body No. 1 of Example 1.
- a sintered body was produced in the same manner as in No. 3 (this sintered body is referred to as “sintered body No. 601” for convenience).
- the first material A is based on a paper published in 2011 (J. Jpn. Soc. Powder Powder Metallurgy, Vol. 58, No. 12, P727-732) and the following method (sol-gel method). ).
- the precursor washed is dried at 120 ° C. in a vacuum to obtain a precursor.
- the mixing ratio is 1.5 mol% Y 2 O 3 and 25 mol% Al 2 O 3 with respect to ZrO 2 .
- the precursor (powder) thus obtained was calcined (heat treated) at 700 ° C. in air for 9 hours, and further calcined at 900 ° C. for 1 hour to obtain the crystalline material as the first material A ZrO 2 (Al 2 O 3 , Y 2 O 3 solid solution) powder is obtained.
- the first material A is partially stabilized ZrO 2 in which 30% by volume of Al 2 O 3 is solid-solved with respect to the entire first material.
- the above sintered body No. Except for replacing the first material A (content: 40% by volume) in 601 with 23% by volume of the first material A and 17% by volume of the third phase and / or the fourth phase described in Table 6, Other than the above, the sintered body No. Sixteen kinds of sintered bodies were produced in the same manner as in the case of the 601 (sintered bodies No. 602 to No. 617).
- the location of Al 2 O 3 in the first material is specified by the same method as in Example 1, and the equivalent circle diameter (particle size) of Al 2 O 3 and the content are included.
- the sintered body No. 3 was confirmed to be the same.
- the region of cBN, the first material, the third phase, and the fourth phase is obtained by a reflected electron image obtained by measuring the CP processed surface of each sintered body with a scanning electron microscope (SEM) or by elemental analysis by Auger electron spectroscopy. Then, when the area was measured by binarization processing using the above image analysis software, the composition and content of cBN, the first material, the third phase, and the fourth phase were as described above and Table 6. It was confirmed that it was the same as described.
Abstract
Description
最初に本発明の実施態様を列記して説明する。
以下、本発明の実施形態(以下「本実施形態」とも記す)についてさらに詳細に説明する。
従来、cBNと、Al2O3およびZr化合物等とを含んだ焼結体は、それを切削工具として用いた場合、遠心鋳造鋳鉄の高速切削において良好な耐摩耗性を有することが知られていた。しかし、Al2O3は低靭性材料であるため、高速の長距離切削に用いた際、欠損する場合があり課題とされていた。
<第1材料>
第1材料は、5~90体積%のAl2O3が結晶粒界または結晶粒内に分散した部分安定化ZrO2である。換言すれば、第1材料は、5~90体積%のAl2O3が部分安定化ZrO2の結晶粒界または結晶粒内に分散した複合酸化物である。
中和共沈法とは、以下の工程Aおよび工程Bを含む方法である。このような方法は、たとえば2013年に発表された論文(J. Jpn. Soc. Powder Powder Metallurgy,Vol.60,No.10,P428-435)に記載されている。
ゾル-ゲル法とは、以下の工程Xを含む方法である。このような方法は、たとえば2011年に発表された論文(J. Jpn. Soc. Powder Powder Metallurgy,Vol.58,No.12,P727-732)に記載されている。
本実施形態の第1材料は、上記の2方法以外の方法によっても得ることができる。すなわち、部分安定化ZrO2とAl2O3とをビーズミルまたはボールミルのような粉砕機を用いてエタノール等の溶媒中で混合しスラリーを得る。次いで、このスラリーを用いて造粒することにより第1材料を得ることができる。造粒手段は特に限定されず、溶融造粒、噴霧造粒等を挙げることができる。
(1)熱処理炉(たとえば1000℃、真空中、3時間)で焼結する。
(2)造粒物の前駆段階の上記スラリーにバインダー(たとえば一般的バインダーであるPVB(ポリビニルブチラール))を10質量%添加する。
本実施形態の焼結体に含まれる立方晶窒化ホウ素は、0.1~5μmの平均粒径を有することが好ましい。0.1μm未満の場合、他の粉末と混合する際、凝集しやすいため焼結不良となる傾向があり、5μmを超えると、焼結時粒成長により強度が低下する傾向がある。
本実施形態の焼結体は、上記の第1材料および立方晶窒化ホウ素以外に、さらに第3相を含むことができる。このような第3相は、酸化アルミニウム、酸化マグネシウム、酸化セリウム、酸化イットリウム、酸化ハフニウム、およびZrOからなる群より選ばれる少なくとも1種であることが好ましい。焼結体がこのような第3相を含むことにより、焼結性が向上し、焼結体の強度がさらに向上する。
本実施形態の焼結体は、上記の第1材料および立方晶窒化ホウ素以外に、さらに第4相を含むことができる。第4相は、上記の第3相とともに焼結体中に含まれていても良い。
本実施形態の焼結体は、従来公知の製造方法により製造することができ、特にその製造方法が限定されるものではない。
本実施形態の焼結体は、上記のように優れた耐欠損性、耐摩耗性等の特性を示すため切削工具などに用いることが好適である。すなわち、本実施形態の切削工具は、上記の焼結体を含むものである。
原料として、60体積%のcBNと40体積%の第1材料とを準備した。cBNは平均粒径2μmであり、第1材料は下記のように中和共沈法により作製されたものであって、第1材料全体に対して30体積%のAl2O3が固溶した部分安定化ZrO2であり、粒径は0.01μmであった。
第1材料は、前述の通り、2013年に発表された論文(J. Jpn. Soc. Powder Powder Metallurgy,Vol.60,No.10,P428-435)に基づき下記の方法により作製できる。
切削速度:900m/min
送り:0.2mm
切込み:0.3mm
湿式/乾式:湿式(クーラント:エマルジョン)
装置:LB4000(オークマ社製)
被削材:遠心鋳造鋳鉄(緻密パーライト、デンドライト組織等を有するFC250(ネズミ鋳鉄))
被削材の形状:円筒状(外径φ95mm)
(切削試験)
10.0km切削後の逃げ面摩耗量(μm)を測定するとともに、12.0km切削後の摩耗形態および欠損状況を観察した。その結果を表1に示す。
上記で準備した第1材料(前駆体)のみを用いて、焼結温度を表1記載の温度とすることを除き、他は全て上記と同様にして焼結体No.7~焼結体No.10の4種の焼結体を得た。そして上記と同様にして切削試験を行なった。
焼結体中の第1材料の含有量を以下の表2の通り変更することを除き、他は全て実施例1の焼結体No.3(すなわち焼結温度が1500℃のもの)と同様にして、7種類の焼結体を作製した(焼結体No.3a、No.3b、No.3c、No.3d、No.3e、No.3f、No.3g)。
<実施例3>
第1材料中のAl2O3の含有量を以下の表3の通り変更することを除き、他は全て実施例1の焼結体No.3と同様にして、7種類の焼結体を作製した(焼結体No.3t、No.3u、No.3v、No.3w、No.3x、No.3y、No.3z)。
焼結体中の第1材料(含有量:40体積%)を、23体積%の第1材料と17体積%の表4記載の第3相および/または第4相とに置き換えることを除き、他は全て実施例1の焼結体No.3と同様にして、24種類の焼結体を作製した(焼結体No.301~No.324)。
<実施例5>
焼結体中の第1材料(含有量:40体積%)を、以下の第1材料(1)~第1材料(6)にそれぞれ置き換えることを除き、他は全て実施例1の焼結体No.3と同様にして、6種類の焼結体を作製した。
部分安定化ZrO2粉末(商品名:「TZ-3Y」、東ソー製、平均粒径:45nm)とAl2O3粉末(商品名:「TM-DAR」、大明化学製、平均粒径:0.1μm)とを、溶媒(エタノール)中でボールミルを用いて混合し、混合スラリーを得た。なお、両粉末の混合割合は、焼結体中での含有割合がZrO2が34体積%、Al2O3が6体積%(第1材料中に占める割合:15体積%)となるように混合した。
部分安定化ZrO2粉末とAl2O3粉末とを、焼結体中での含有割合がZrO2が28体積%、Al2O3が12体積%(第1材料中に占める割合:30体積%)となるように混合することを除き、他は全て第1材料(1)と同様にして第1材料(2)を得た。
部分安定化ZrO2粉末とAl2O3粉末とを、焼結体中での含有割合がZrO2が20体積%、Al2O3が20体積%(第1材料中に占める割合:50体積%)となるように混合することを除き、他は全て第1材料(1)と同様にして第1材料(3)を得た。
部分安定化ZrO2粉末(商品名:「TZ-3Y」、東ソー製、平均粒径:45nm)とAl2O3粉末(商品名:「TM-DAR」、大明化学製、平均粒径:0.1μm)とを、バインダーとしてポリビニルブチラール(商品名:「エスレックB」、積水化学工業株式会社製)を10質量%添加した溶媒(エタノール)中でボールミルを用いて混合し、混合スラリーを得た。なお、両粉末の混合割合は、焼結体中での含有割合がZrO2が34体積%、Al2O3が6体積%(第1材料中に占める割合:15体積%)となるように混合した。
部分安定化ZrO2粉末とAl2O3粉末とを、焼結体中での含有割合がZrO2が28体積%、Al2O3が12体積%(第1材料中に占める割合:30体積%)となるように混合することを除き、他は全て第1材料(4)と同様にして第1材料(5)を得た。
部分安定化ZrO2粉末とAl2O3粉末とを、焼結体中での含有割合がZrO2が20体積%、Al2O3が20体積%(第1材料中に占める割合:50体積%)となるように混合することを除き、他は全て第1材料(4)と同様にして第1材料(6)を得た。
<実施例6>
焼結体中の第1材料を、以下のようにして作製した第1材料(この第1材料を便宜上「第1材料A」とする)に置き換えること(すなわち焼結体原料の第1材料前駆体を以下の「第1材料A」に置き換えること)を除き、他は全て実施例1の焼結体No.3と同様にして、焼結体を作製した(この焼結体を便宜上「焼結体No.601」とする)。
第1材料Aは、前述の通り、2011年に発表された論文(J. Jpn. Soc. Powder Powder Metallurgy,Vol.58,No.12,P727-732)に基づき下記の方法(ゾル-ゲル法)により作製できる。
以上のように本発明の実施の形態および実施例について説明を行なったが、上述の各実施の形態および実施例の構成を適宜組み合わせたり、様々に変形することも当初から予定している。
Claims (11)
- 第1材料と立方晶窒化ホウ素とを含む焼結体であって、
前記第1材料は、5~90体積%のAl2O3が結晶粒界または結晶粒内に分散した部分安定化ZrO2である、焼結体。 - 前記第1材料は、5~50体積%のAl2O3が結晶粒界または結晶粒内に分散した部分安定化ZrO2である、請求項1に記載の焼結体。
- 前記第1材料は、50体積%超70体積%以下のAl2O3が結晶粒界または結晶粒内に分散した部分安定化ZrO2である、請求項1に記載の焼結体。
- 前記第1材料は、70体積%超90体積%以下のAl2O3が結晶粒界または結晶粒内に分散した部分安定化ZrO2である、請求項1に記載の焼結体。
- 前記Al2O3は、その粒径が1μm以下の粒子である、請求項1~請求項4のいずれか1項に記載の焼結体。
- 前記Al2O3は、その粒径が0.5μm以下の粒子である、請求項5に記載の焼結体。
- 前記Al2O3は、その粒径が0.1μm以下の粒子である、請求項6に記載の焼結体。
- 前記焼結体は、20~80体積%の前記第1材料を含む、請求項1~請求項7のいずれか1項に記載の焼結体。
- 前記焼結体は、さらに第3相を含み、
前記第3相は、酸化アルミニウム、酸化マグネシウム、酸化セリウム、酸化イットリウム、酸化ハフニウム、およびZrOからなる群より選ばれる少なくとも1種である、請求項1~請求項8のいずれか1項に記載の焼結体。 - 前記焼結体は、さらに第4相を含み、
前記第4相は、周期表の4族元素、5族元素、6族元素、Al、およびSiからなる群より選ばれる少なくとも1種の元素と、炭素、窒素、およびホウ素からなる群より選ばれる少なくとも1種の元素とからなる少なくとも1種の化合物である、請求項1~請求項9のいずれか1項に記載の焼結体。 - 請求項1~請求項10のいずれか1項に記載の焼結体を含む切削工具。
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