JP4976602B2 - アルミナ質焼結体、砥粒、及び砥石 - Google Patents
アルミナ質焼結体、砥粒、及び砥石 Download PDFInfo
- Publication number
- JP4976602B2 JP4976602B2 JP2012503809A JP2012503809A JP4976602B2 JP 4976602 B2 JP4976602 B2 JP 4976602B2 JP 2012503809 A JP2012503809 A JP 2012503809A JP 2012503809 A JP2012503809 A JP 2012503809A JP 4976602 B2 JP4976602 B2 JP 4976602B2
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- JP
- Japan
- Prior art keywords
- alumina
- sintered body
- powder
- alumina sintered
- abrasive grains
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims description 90
- 239000006061 abrasive grain Substances 0.000 title claims description 33
- 239000013078 crystal Substances 0.000 claims description 38
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 29
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 19
- 150000002506 iron compounds Chemical class 0.000 claims description 14
- 150000003609 titanium compounds Chemical class 0.000 claims description 13
- 239000000843 powder Substances 0.000 description 63
- 239000002245 particle Substances 0.000 description 20
- 238000000227 grinding Methods 0.000 description 19
- 238000000034 method Methods 0.000 description 19
- 239000000203 mixture Substances 0.000 description 19
- 230000001186 cumulative effect Effects 0.000 description 18
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 15
- 239000002994 raw material Substances 0.000 description 15
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 description 13
- 238000009863 impact test Methods 0.000 description 11
- 239000000463 material Substances 0.000 description 10
- 229910052719 titanium Inorganic materials 0.000 description 10
- 229940043430 calcium compound Drugs 0.000 description 9
- 150000001674 calcium compounds Chemical class 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 9
- 150000003377 silicon compounds Chemical class 0.000 description 9
- 239000010936 titanium Substances 0.000 description 9
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 239000000292 calcium oxide Substances 0.000 description 8
- 229910052742 iron Inorganic materials 0.000 description 8
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 8
- 229910044991 metal oxide Inorganic materials 0.000 description 8
- 150000004706 metal oxides Chemical class 0.000 description 8
- 239000002002 slurry Substances 0.000 description 8
- 229910004298 SiO 2 Inorganic materials 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000002131 composite material Substances 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- 229910052593 corundum Inorganic materials 0.000 description 5
- 239000010431 corundum Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000010304 firing Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000005530 etching Methods 0.000 description 4
- 235000013980 iron oxide Nutrition 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 150000002736 metal compounds Chemical class 0.000 description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 238000007088 Archimedes method Methods 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000003082 abrasive agent Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 239000010953 base metal Substances 0.000 description 2
- 238000011088 calibration curve Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000004070 electrodeposition Methods 0.000 description 2
- 230000002706 hydrostatic effect Effects 0.000 description 2
- 238000007561 laser diffraction method Methods 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 229910052861 titanite Inorganic materials 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910002012 Aerosil® Inorganic materials 0.000 description 1
- 229910002016 Aerosil® 200 Inorganic materials 0.000 description 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910000505 Al2TiO5 Inorganic materials 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 229910052661 anorthite Inorganic materials 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000009694 cold isostatic pressing Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- GWWPLLOVYSCJIO-UHFFFAOYSA-N dialuminum;calcium;disilicate Chemical compound [Al+3].[Al+3].[Ca+2].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] GWWPLLOVYSCJIO-UHFFFAOYSA-N 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 229910001678 gehlenite Inorganic materials 0.000 description 1
- 239000003966 growth inhibitor Substances 0.000 description 1
- 238000007542 hardness measurement Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- IXQWNVPHFNLUGD-UHFFFAOYSA-N iron titanium Chemical compound [Ti].[Fe] IXQWNVPHFNLUGD-UHFFFAOYSA-N 0.000 description 1
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000009719 polyimide resin Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- AABBHSMFGKYLKE-SNAWJCMRSA-N propan-2-yl (e)-but-2-enoate Chemical compound C\C=C\C(=O)OC(C)C AABBHSMFGKYLKE-SNAWJCMRSA-N 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910001256 stainless steel alloy Inorganic materials 0.000 description 1
- 229920006337 unsaturated polyester resin Polymers 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D3/00—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
- B24D3/34—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents characterised by additives enhancing special physical properties, e.g. wear resistance, electric conductivity, self-cleaning properties
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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
- C04B35/01—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
- C04B35/10—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 aluminium oxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D3/00—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D3/00—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
- B24D3/02—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent
- B24D3/04—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially inorganic
- B24D3/06—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially inorganic metallic or mixture of metals with ceramic materials, e.g. hard metals, "cermets", cements
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- C04B35/1115—Minute sintered entities, e.g. sintered abrasive grains or shaped particles such as platelets
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62625—Wet mixtures
- C04B35/6263—Wet mixtures characterised by their solids loadings, i.e. the percentage of solids
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1409—Abrasive particles per se
- C09K3/1418—Abrasive particles per se obtained by division of a mass agglomerated by sintering
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3427—Silicates other than clay, e.g. water glass
- C04B2235/3463—Alumino-silicates other than clay, e.g. mullite
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Description
研削比=被削材が削られた量(研削量)/砥石の摩耗量
(1)砥粒の硬度が高くなると研削量が増えるため研削比は大きくなる。
(2)破壊靱性が高くなると砥粒の摩耗量が少なくなるため研削比は大きくなる。
[1] チタン化合物及び鉄化合物を含むアルミナ質焼結体であって、アルミナ結晶の粒界にFeTiAlO5の結晶が存在し、該FeTiAlO5結晶の平均結晶サイズが3.4〜7.0μmであるアルミナ質焼結体。
[2] チタン化合物をTiO2に換算した含有量と鉄化合物をFe2O3に換算した含有量との合計量が5〜13質量%である請求項1に記載のアルミナ質焼結体。
[3] 上記[1]又は上記[2]に記載のアルミナ質焼結体からなる砥粒。
[4] 上記[3]に記載の砥粒の層を作用面に有する砥石。
本発明のアルミナ質焼結体においては、コランダム結晶から構成される主結晶相の粒界に、Ti、Fe及びAlを含む複合金属酸化物の結晶相、具体的にはFeTiAlO5粒子が存在する。このFeTiAlO5粒子の存在により、高硬度で破壊靭性に優れた砥粒を与えるアルミナ質焼結体となる。特に、FeTiAlO5粒子は、コランダム相よりも破壊靭性が高いといった作用により、高硬度で破壊靭性に優れたアルミナ質焼結体が得られる。FeTiAlO5粒子からなる結晶相の存在及び平均結晶サイズは、後述の実施例に記載の方法により確認することができる。
3.4〜7.0μmの範囲外では破壊時に生じるクラックの進行を抑制する効果が小さくなる。逆に、平均結晶サイズが3.4〜7.0μmの範囲にあることで、当該FeTiAlO5粒子によるクラックの偏向効果を良好に保つことができる。
まず、アルミナだけからなる焼結体の場合は、図3に示すように、クラックの伝わり方は、アルミナ粒子12の粒界に沿って矢印Y方向に進行することになる。そして、衝撃の大きさによっては、図4(B)のSEM写真に示すように、粒界に沿って直線的に亀裂が生じることになる。なお、図4は、後述の比較例1に係る焼結体のSEM写真であり、図4(A)は衝撃を加える前の結晶組織の様子を示し、図4(B)は衝撃を加えた後のクラック伝播の様子を示す。
このことは、図2に示す衝撃試験の結果を示すSEM写真からもわかる。すなわち、図2(A)のSEM写真のようにアルミナ粒子の粒界にFeTiAlO5粒子が存在する状態で衝撃を加えると、図2(B)のようにクラックはFeTiAlO5粒子を起点にこれを迂回するように進行する。
なお、図2は後述の実施例3に係る焼結体のSEM写真であり、当該図中、アルミナ粒子の粒界にある三重点に位置する灰色部分(色の薄い部分)がFeTiAlO5粒子に相当する。
また、TiO2換算含有量とFe2O3換算含有量との2成分合計量が5〜13質量%となっていることが好ましく、7〜10質量%となっていることがより好ましい。
ケイ素化合物をSiO2換算した含有量(以下、「SiO2換算含有量」ということがある)とカルシウム化合物をCaO換算した含有量(以下、「CaO換算含有量」ということがある)との合計量は2質量%以下となっていることが好ましく、0.5〜2質量%となっていることがより好ましい。
ケイ素化合物及びカルシウム化合物は粒成長剤として作用し、これらが酸化物換算で2質量%以下存在することで、アルミナのコランダム結晶の形状・サイズを不均一にし、クラックの偏向を生じさせるものと考えられる。つまり、特定量のチタン化合物及び鉄化合物、及び特定量のケイ素化合物及びカルシウム化合物の存在により、それぞれの作用が組み合わさってクラックの偏向が効率よく生じ、より高い破壊靭性化の効果が得られると考えられる。
まず測定を行うために、元素の組成が既知の標準酸化物試料の湿式分析を行う。得られた湿式分析値を基準値として、測定の際に必要な検量線を作成する。サンプルの定量分析は、この作成した検量線を基に行う。測定機器としては、Panalytical社製、「PW2400型」を用いることができる。また測定は、管球:ロジウム管球、特性X線:Kα線の条件で実施することが好ましい。管電圧及び管電流は元素ごとに異なる条件で測定を行うことが好ましい。管電圧と管電流の条件の一例を下記表1に示す。
なお、本明細書において、各金属酸化物換算含有量を求める際の分母となる全体量は、アルミナ質焼結体に含まれる全ての金属元素を酸化物に換算して合計した量となる。
次に、既述の本発明のアルミナ質焼結体の製造方法について説明する。
(原料)
本発明のアルミナ質焼結体の製造方法においては、原料としてアルミナ、チタン化合物、鉄化合物を用いる。必要に応じてさらにケイ素化合物及び/又はカルシウム化合物を用いる。これらは2種以上を含む複合酸化物でもよい。
ここで、各種粉末の累積質量50%径(d50)は、レーザー回折法により測定することができる。
ケイ素化合物粉末、カルシウム化合物粉末としては、それぞれ高純度のSiO2粉末及び高純度のCaO粉末、炭酸カルシウム粉末等であってもよいし、シリカ、酸化カルシウム、アルミナの全部あるいはそれらの中の2種が複合酸化物を形成したものであってもよい。複合酸化物としては、ムライト、ゼオライト、ベントナイト、ゲーレナイト、アノーサイト等の粉末が挙げられる。
本発明のアルミナ質焼結体を製造する方法において、原料の混合物を調製する方法に特に制限はないが、例えば下記の方法を好ましく採用することができる。
まず、ポリビニルアルコールを含む水性媒体中に、バイヤー法で得られたアルミナ粉末、イルメナイト粉末(又はTiO2粉末とFe2O3粉末)を、それぞれ所定量を加える。その後、例えば、超音波分散機、遊星ボールミル、ボールミル、サンドミル等のメディアを用いた分散機、アルティマイザー(商品名)、ナノマイザー(商品名)等のメディアレス分散機等を用いて均質なスラリーを得る。次いで、このスラリーを乾燥処理したのち、粉砕して、累積質量50%径(d50)3μm以下、好ましくは1μm以下の混合物(粉末)を調製する。
上記のようにして調製された原料の混合物の成形体を焼結して、相対密度95%以上、好ましくは97%以上である本発明のアルミナ質焼結体を得る。相対密度が95%以上であることで、焼結体中の気孔・空隙に起因する焼結体硬度および破壊靭性の低下を抑制することができる。なお、相対密度はアルキメデス法で測定した焼結嵩密度を真密度で除して求めることができる。
また、焼結に際しては、公知の成形手段、例えば金型プレス、冷間静水圧プレス、鋳込成形、射出成形、押出し成形等により任意の形状に成形し、次いでこの成形体を公知の焼結法、例えば、ホットプレス法、常圧焼成法、ガス加圧焼成法、マイクロ波加熱焼成法等、種々の焼結手法によって焼結してもよい。
本発明の砥粒は、本発明のアルミナ質焼結体からなる。本発明のアルミナ質焼結体は、粉砕処理、混練処理、成形処理、乾燥処理、焼結処理を順次施すことで得られる。
本発明の砥石は、本発明の砥粒の層を作用面に有するものである。
本発明の砥石における砥粒の作用面への固定方法としては、レジンボンド、ビトリファイドボンド、メタルボンド、電着等が挙げられる。
また、台金の材質としては、スチール、ステンレス合金、アルミニウム合金等が挙げられる。
以上に鑑み、砥石においては、その用途に応じて砥粒の固定方法が選択される。
本発明の砥石の形状については特に制限はなく、砥石の用途に応じて、ストレート型やカップ型等の形状から適宜選択すればよい。
なお、各例における諸特性は以下に示す方法に従って求めた。
原料粉末の累積質量50%径(d50)は、レーザー回折法(日機装(株)製 マイクロトラック HRA)により測定した。
装置として(株)アカシ製、機種名「MVK−VL、Hardness Tester」を用い、測定は、荷重0.98N、圧子の打ち込み時間10秒の条件とし、15点の測定値の平均値を平均ビッカース硬度とした。平均ビッカース硬度が16GPa以上であれば実用上問題ない。
装置として松沢精機株式会社製、機種名「DVK−1」を用い、測定は、最大荷重9.81N、圧子の打ち込み速度50μm/sec、圧子の打ち込み時間15秒の条件にて15点の平均値を平均破壊靱性値とした。計算式は以下の通りである。また、平均破壊靱性値が3.0MPa・m1/2以上であれば実用上問題ない。
KIC = 0.026 * E1/2 * P1/2 * a / c3/2
KIC : 破壊靱性値(MPa・m1/2)
E : ヤング率(Pa)
P : 最大荷重(N)
a : 圧痕寸法(m)
c : クラックの寸法(m)
なお、本発明において上記ヤング率Eは、アルミナの値(3.9×1011Pa)を用いた。
装置として日本電子(株)製、機種名「JSM−6510V」を用いてSEM写真を撮影した。得られたSEM写真から各結晶相の平均結晶サイズを測定した。平均結晶サイズは、各結晶(50個)の同一方向における最大長さを直径法により測定し、平均を算出して求めた。
装置としてPanalytical社製、機種名「X'pert PRO」を用い、特性X線:CuKα線、管電圧40kV、管電流40mAの条件にて上記金属酸化物結晶相の組成分析を行った。
相対密度はアルキメデス法で測定した各焼結体の嵩密度を真密度で除して求めた。
この際、添加した鉄化合物とチタン化合物とは全て反応してFeTiAlO5になったと仮定し、その上で、アルミナの真密度を3.98、FeTiAlO5の真密度を4.28とし、生成され得るFeTiAlO5の割合と残部であるアルミナの割合をもとに真密度を算出した。
累積質量50%径(d50)0.6μmの上記アルミナ粉末と、累積質量50%径(d50)0.75μmの上記イルメナイト粉末とを、形成されるアルミナ質焼結体中のTiO2及びFe2O3の各含有量が表9−1及び表9−2に示す値となるように混合して各種混合物を得た。
また、図2に実施例3のアルミナ質焼結体に対する衝撃試験前後のSEM写真を、図4に、比較例1のアルミナ質焼結体に対する衝撃試験前後のSEM写真を示す。なお、これらの図中、(A)は衝撃試験前の結晶組織の様子を示し、(B)は衝撃試験後のクラック伝播の様子を示す。
累積質量50%径(d50)0.6μmの上記アルミナ粉末と、累積質量50%径(d50)0.5μmの酸化鉄粉末、及び累積質量50%径(d50)0.6μmの酸化チタン粉末を、形成されるアルミナ質焼結体中のTiO2及びFe2O3の各含有量が表9−1及び表9−2に示す値となるように混合して各種混合物を得た。
次いで、この各種スラリーを、それぞれ120℃で24時間乾燥処理した後、乳鉢により解砕処理して、累積質量50%径(d50)300μm以下の各種粉砕品を得た。この各種粉砕品を、それぞれ100MPaの圧力で金型成形したのち、さらに150MPaの圧力で静水圧処理を施して各種成形体を作製した。
次に、この各種成形体を相対密度が95%以上になるように、電気炉(大気雰囲気)にて4時間焼成することにより各種のアルミナ質焼結体を得た。これらについて、既述のような試験(評価)を行った。結果を下記表9−1及び表9−2に示す。
X線回折測定のデータ解析は、PANalytical社製の解析ソフト「X’Pert High Score Plus」を用いて行った。
この解析ソフトでは、FeAlTiO5の構造を、1982年にTiedemann等が発表した文献を基に結晶構造を決定した。
それによって得られたパターンと、実験サンプルの結果を照合して、ピークがFeAlTiO5に起因するものであると判断した。
12:アルミナ粒子
X :クラックの進行方向を示す矢印
Y :クラックの進行方向を示す矢印
Claims (4)
- チタン化合物及び鉄化合物を含むアルミナ質焼結体であって、アルミナ結晶の粒界にFeTiAlO5の結晶が存在し、該FeTiAlO5結晶の平均結晶サイズが3.4〜7.0μmであるアルミナ質焼結体。
- チタン化合物をTiO2に換算した含有量と鉄化合物をFe2O3に換算した含有量との合計量が5〜13質量%である請求項1に記載のアルミナ質焼結体。
- 請求項1に記載のアルミナ質焼結体からなる砥粒。
- 請求項3に記載の砥粒の層を作用面に有する砥石。
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