WO2010058745A1 - Alumine colorée frittée de dureté et translucidité élevées, et procédé de fabrication et ses utilisations - Google Patents
Alumine colorée frittée de dureté et translucidité élevées, et procédé de fabrication et ses utilisations Download PDFInfo
- Publication number
- WO2010058745A1 WO2010058745A1 PCT/JP2009/069393 JP2009069393W WO2010058745A1 WO 2010058745 A1 WO2010058745 A1 WO 2010058745A1 JP 2009069393 W JP2009069393 W JP 2009069393W WO 2010058745 A1 WO2010058745 A1 WO 2010058745A1
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- Prior art keywords
- alumina
- sintered body
- oxide
- group
- metal oxide
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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 abstract description 104
- 238000004519 manufacturing process Methods 0.000 title claims description 22
- 239000002245 particle Substances 0.000 claims abstract description 46
- 229910000314 transition metal oxide Inorganic materials 0.000 claims abstract description 35
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 claims abstract description 16
- 229910000272 alkali metal oxide Inorganic materials 0.000 claims abstract description 13
- 238000002834 transmittance Methods 0.000 claims abstract description 13
- 239000005548 dental material Substances 0.000 claims abstract description 9
- 230000005496 eutectics Effects 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 20
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 18
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 18
- 238000001513 hot isostatic pressing Methods 0.000 claims description 17
- 238000005245 sintering Methods 0.000 claims description 16
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 14
- 229910005793 GeO 2 Inorganic materials 0.000 claims description 12
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 8
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 claims description 8
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 8
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 8
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 8
- 229910001935 vanadium oxide Inorganic materials 0.000 claims description 8
- 239000005751 Copper oxide Substances 0.000 claims description 7
- 229910000431 copper oxide Inorganic materials 0.000 claims description 7
- 239000010419 fine particle Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract 2
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 abstract 2
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 abstract 2
- 229910011255 B2O3 Inorganic materials 0.000 abstract 1
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 abstract 1
- 229910044991 metal oxide Inorganic materials 0.000 abstract 1
- 150000004706 metal oxides Chemical class 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 11
- 238000005452 bending Methods 0.000 description 10
- 239000011148 porous material Substances 0.000 description 8
- 238000004040 coloring Methods 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 6
- 229910000423 chromium oxide Inorganic materials 0.000 description 6
- 229910000428 cobalt oxide Inorganic materials 0.000 description 6
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 6
- 239000000395 magnesium oxide Substances 0.000 description 6
- 238000012545 processing Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- -1 B 2 O 3 Chemical compound 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000000280 densification Methods 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000004115 Sodium Silicate Substances 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000003486 chemical etching Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(iii) oxide Chemical compound O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 description 2
- 238000007656 fracture toughness test Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 230000000737 periodic effect Effects 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 235000019795 sodium metasilicate Nutrition 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 229910052911 sodium silicate Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 238000007088 Archimedes method Methods 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 101100371219 Pseudomonas putida (strain DOT-T1E) ttgE gene Proteins 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- ODDFFGFVNFSWQX-UHFFFAOYSA-N [O-2].[V+5].[Ni]=O.[O-2].[O-2].[O-2].[O-2].[V+5] Chemical compound [O-2].[V+5].[Ni]=O.[O-2].[O-2].[O-2].[O-2].[V+5] ODDFFGFVNFSWQX-UHFFFAOYSA-N 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 235000019219 chocolate Nutrition 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 229910052805 deuterium Inorganic materials 0.000 description 1
- 229910001940 europium oxide Inorganic materials 0.000 description 1
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000010437 gem Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000003966 growth inhibitor Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000010191 image analysis Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000000879 optical micrograph Methods 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 1
- 239000010979 ruby Substances 0.000 description 1
- 229910001750 ruby Inorganic materials 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 238000007569 slipcasting Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 239000012780 transparent material Substances 0.000 description 1
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical class [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 description 1
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
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- A61L27/105—Ceramics or glasses containing Al2O3
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- 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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Definitions
- the present invention relates to a colored alumina sintered body having high toughness and excellent translucency. It can be used for dental materials such as orthodontic brackets and dental restoration mill blanks that require high toughness as well as decorative, jewelry and craft applications.
- translucent alumina sintered bodies have been used not only for decorative products, jewelry and crafts, but also as dental materials such as orthodontic brackets and dental restoration mill blanks.
- dental materials such as orthodontic brackets and dental restoration mill blanks.
- aesthetic properties based on translucency but also improvement of mechanical properties such as fracture toughness are important issues in translucent alumina sintered bodies.
- toughness of translucent alumina sintered bodies hereinafter referred to as colored translucent alumina sintered bodies
- Colored translucent alumina has long been manufactured by Bernoulli method, chocolate lasky method, etc. as artificial gems such as ruby and sapphire. However, since these production methods can obtain a single crystal, it is necessary to machine the single crystal in actual use.
- Patent Documents 1 to 6 disclose a method in which transition metal oxides such as chromium oxide, cobalt oxide and iron oxide are mixed with alumina powder and the powder is molded and sintered.
- Patent Document 1 discloses a method in which alumina powder is mixed with cobalt oxide, nickel oxide, chromium oxide, manganese oxide or the like and sintered in a hydrogen or vacuum atmosphere.
- Patent Document 2 discloses a colored translucent alumina sintered body by hot isostatic pressing (HIP) using a transition metal such as iron oxide, titanium oxide, vanadium oxide, nickel oxide, chromium oxide, and cobalt oxide.
- HIP hot isostatic pressing
- a manufacturing method is disclosed. By these methods, colored translucent alumina sintered bodies such as blue, green, yellow, and pink are obtained.
- the conventional method for producing a colored translucent alumina sintered body is in accordance with a method for producing hydrogen in a vacuum atmosphere (for example, Patent Document 7) or a method using HIP (for example, Patent Document 8).
- the fracture toughness values of colored translucent alumina sintered bodies produced by these methods are as low as about 3 to 4 MPa ⁇ m 0.5 (Patent Document 8), and mechanical properties are required. The high fracture toughness value required for the application was not obtained.
- Patent Document 9 Non-Patent Document 1
- Patent Document 10 anisotropic grain growth of alumina particles
- the present invention provides a colored alumina sintered body having both high toughness and translucency and a method for producing the same.
- the present inventors have obtained a sintered particle structure having anisotropic particles using a transition metal oxide.
- the inventors have found that a sintered body having excellent aesthetic coloration, excellent translucency, and high fracture toughness can be obtained, and the present invention has been completed.
- the gist of the present invention resides in the following (1) to (16).
- (1) The maximum value of the total light transmittance of a sample having a transition metal oxide, a fracture toughness of 4.5 MPa ⁇ m 0.5 or more, and a thickness of 1 mm for light having a wavelength of 300 to 800 nm is 60% or more.
- the alumina sintered body according to (1) or (2), wherein the sintered particles preferably include anisotropic particles having a major axis length of 10 ⁇ m or more and an aspect ratio of 1.5 or more. .
- the alumina sintered body according to (3) wherein the ratio of anisotropic particles having a major axis length of 10 ⁇ m or more and an aspect ratio of 1.5 or more is 20 vol% or more.
- the transition metal oxide having an eutectic point with alumina is at least one selected from the group consisting of manganese oxide, copper oxide, vanadium oxide, iron oxide, titanium oxide, and nickel oxide.
- at least one selected from the group consisting of group 1A alkali metal oxide, group 2A alkaline earth metal oxide, and SiO 2 , B 2 O 3 , P 2 O 5 , GeO 2 is 20
- Alumina sintering characterized by forming an alumina powder containing a total amount of transition metal oxides in the range of 100 ppm to 3 wt%, sintering at normal pressure, and then performing hot isostatic pressing (HIP) treatment Body manufacturing method.
- the transition metal oxide is at least one selected from the group consisting of manganese oxide, copper oxide, vanadium oxide, iron oxide, titanium oxide, and nickel oxide.
- the alumina powder is further selected from the group consisting of Group 1A alkali metal oxide, Group 2A alkaline earth metal oxide, and SiO 2 , B 2 O 3 , P 2 O 5 , GeO 2.
- a high-purity alumina powder having a specific surface area of 5 to 20 m 2 / g and a fine particle ratio of 1 ⁇ m or less of 90 vol% or more is used, according to any one of (9) to (11) Production method.
- HIP hot isostatic pressing
- the conventional colored translucent alumina sintered body has low toughness and lacks chipping during processing and impact resistance when stress is applied.
- the alumina sintered body of the present invention has high aesthetic coloring and translucency, and has high toughness as compared with the prior art, so that it has excellent workability and is not particularly chipped or cracked.
- the alumina sintered body of the present invention contains a transition metal oxide.
- the content of the transition metal oxide in the present invention is preferably 100 ppm to 3 wt%, particularly preferably 300 ppm to 1 wt%. If the content is less than 100 ppm, the effect of adding a transition metal oxide tends to be weakened. If the content exceeds 3 wt%, the transition metal oxide becomes a solid solution limit in alumina and transition metal oxide particles are precipitated in the sintered body, resulting in a decrease in translucency. It's easy to do.
- Fracture toughness of the sintered body of the present invention is 4.5 MPa ⁇ m 0.5 or more, in particular 5 MPa ⁇ m 0.5 or more, and further preferably not 6 MPa ⁇ m 0.5 or more.
- the sintered body of the present invention has high translucency with a maximum value of total light transmittance at a wavelength of 300 to 800 nm of 60% or more at a sample thickness of 1 mm, 65% or more, particularly 70% or more, and further 75% or more. It is preferable that The bending strength of the sintered body of the present invention is not particularly defined, but is preferably 350 MPa or more, particularly 400 MPa or more, and more preferably 500 MPa or more.
- the evaluation methods of fracture toughness and bending strength are based on the method prescribed in JIS, and all values in the present invention are average values (average fracture toughness, average bending strength).
- the alumina sintered body of the present invention preferably contains anisotropic particles having a major axis length of 10 ⁇ m or more and an aspect ratio of 1.5 or more as sintered particles.
- the aspect ratio of the anisotropic particles is particularly preferably 3 or more. The larger the aspect ratio of the anisotropic particles, the higher the fracture toughness.
- a typical example of the alumina sintered particles constituting the alumina sintered body of the present invention is shown in FIG.
- the content of anisotropic particles in the alumina sintered body of the present invention is preferably 20 vol% or more, particularly 30 vol% or more, and more preferably 50 vol% or more. As the content of anisotropic particles increases, the fracture toughness of the sintered body increases. On the other hand, when the anisotropic particle content is close to 100 vol%, the fracture toughness reaches 10 MPa ⁇ m 0.5 or more, but the bending strength tends to decrease to 300 MPa or less. Need not increase excessively.
- the anisotropic particles in the alumina sintered body of the present invention are particularly preferably plate-shaped (anisotropic plate-shaped particles).
- the sintered structure of the alumina sintered body of the present invention is composed of equiaxed particles other than anisotropic particles, and the anisotropic particles contribute to the improvement of fracture toughness, while the equiaxed particles are anisotropic particles. It works to connect the gaps and contributes to strength maintenance.
- the alumina sintered body of the present invention has high toughness and translucency due to a sintered structure containing specific anisotropic particles, and has a low toughness sintered body containing a conventional auxiliary agent such as magnesium oxide. Is different.
- the transition metal oxide contained in the alumina sintered body of the present invention is preferably a transition metal oxide having a eutectic point with alumina, manganese oxide, copper oxide, vanadium oxide, iron oxide, titanium oxide, oxidation It is particularly preferred that at least one selected from the group of nickel. These transition metal oxides provide a desired color and provide a liquid phase in alumina to promote anisotropic growth of alumina particles.
- the alumina sintered body of the present invention further comprises a group 1A alkali metal oxide, a group 2A alkaline earth metal oxide, and SiO 2 , B 2 O 3 , P 2 O 5 , GeO 2 .
- At least one selected from the group is contained in a total amount of 20 to 1000 ppm.
- 1A group alkali metal oxides such as Na 2 O, 2A group alkaline earth metal oxides and SiO 2 , B 2 O 3 , P 2 O 5 , GeO 2 act as glass phase forming agents, and anisotropic growth of alumina particles Promote.
- oxides having a high glass phase forming ability are Na 2 O and Na 2 O + SiO 2 .
- examples of the group 1A alkali metal of the periodic table include lithium, sodium, potassium, rubidium, and cesium.
- MgO is a group 2A alkaline earth metal oxide.
- the group 1A alkali metal oxidation is performed.
- examples of the group 2A alkaline earth metal of the periodic table include beryllium, magnesium, calcium, strontium, and barium.
- the total content of the components of seeds or more is preferably 20 to 1000 ppm, and if it is less than 20 ppm, the effect is dilute, and if it exceeds 1000 ppm, sintering is inhibited.
- the alumina sintered body of the present invention is at least one selected from the group consisting of group 1A alkali metal oxides, group 2A alkaline earth metal oxides, and SiO 2 , B 2 O 3 , P 2 O 5 , GeO 2. In the range of 20 to 1000 ppm in total, there is no particular limitation on the transition metal oxide, and those that develop the desired color can be used, such as cobalt oxide that develops blue, chromium oxide that develops red, etc. Can be illustrated.
- the sintered body of the present invention is manufactured by forming an alumina powder containing a transition metal oxide in a total amount in the range of 100 ppm to 3 wt%, sintering it at normal pressure, and then subjecting it to hot isostatic pressing (HIP). can do.
- the transition metal oxide is preferably a transition metal oxide having a eutectic point with alumina, and in particular, at least one selected from the group consisting of manganese oxide, copper oxide, vanadium oxide, iron oxide, titanium oxide, and nickel oxide. One or more are preferable.
- the alumina powder is further selected from the group of group 1A alkali metal oxide, group 2A alkaline earth metal oxide, and SiO 2 , B 2 O 3 , P 2 O 5 , GeO 2. It is preferable to contain at least one kind in a range of 20 to 1000 ppm in total. These oxides promote the anisotropic growth of alumina particles. Therefore, when these oxides are contained, the type of transition metal oxide contained in the alumina powder is not limited, and a transition metal oxide having a desired color development can be used.
- the raw material alumina powder to which the different components are added is a high-purity alumina powder having a purity of 99.99% or higher, and a specific surface area of 5 to 20 m 2 / g, a fine particle ratio of 1 ⁇ m or less 90 vol%. What consists of the above fine particle is preferable.
- high-purity alumina powder as a starting material, the content of different components becomes uniform and a high-quality sintered body can be obtained.
- the fine particle ratio of the alumina powder is important, and if it is less than 90 vol%, the temperature for densification increases due to sintering, which is not preferable.
- the above different components may be added to the alumina powder and dispersed by a mixing and / or grinding device.
- the mixing and / or pulverization method may be a wet method using water, ethanol or the like, or a dry method.
- the oxides of the different components can be added as oxide powders, but precursors (chlorides, inorganic acid salts, organic acid salts, etc.) that become oxides upon firing may be added.
- a water-soluble salt such as NaCl can be used. What is necessary is just to mix these raw materials so that it may become a predetermined amount, and to dry and / or bake.
- the method for forming the powder in the production method of the present invention is not particularly limited, and for example, any method such as a die press, rubber press, slip casting, injection molding and the like can be applied.
- an alumina powder molded body having the above composition is fired at normal pressure and then subjected to hot isostatic pressure (HIP) treatment.
- the atmospheric pressure sintering in the production method of the present invention is preferably carried out at a temperature of 1250 ° C. to 1450 ° C. in an atmosphere such as air, oxygen or vacuum.
- the sintered body is densified to the density necessary for the next HIP treatment (about 95% of the theoretical density).
- the pressure medium gas of the HIP treatment penetrates into the sintered body and the removal of pores is not achieved.
- the residual pores in the sintered body be efficiently removed by HIP treatment.
- grain boundary pores are easier to remove than intragranular pores. Therefore, if the sintering temperature of atmospheric sintering is too high, pores are likely to be taken into grains due to grain growth. Removal by processing is difficult. Moreover, the translucency of the sintered compact after HIP processing improves, so that the crystal grain of the primary sintered compact used for HIP processing is finer. Therefore, atmospheric sintering is preferably performed at a temperature of 1250 ° C. to 1450 ° C. from the viewpoint of obtaining a density of 95% or more of the theoretical density, suppressing the formation of intragranular pores, and obtaining fine crystal particles.
- the HIP treatment of the production method of the present invention is performed for the purpose of eliminating residual pores in the sintered body and imparting translucency.
- the treatment temperature is preferably 1200 ° C. or more and the treatment pressure is 50 MPa or more, particularly preferably the temperature is 1300 to 1800 ° C. and the pressure is 100 to 200 MPa. If it is less than 1200 degreeC, the growth of an anisotropic particle is inadequate, and if it exceeds 1800 degreeC, an anisotropic particle will coarsen and it will be difficult to acquire the effect of this invention.
- the treatment temperature is most preferably 1350 to 1750 ° C.
- argon gas As the pressure medium for the HIP process, a commonly used argon gas can be used. Other gases such as nitrogen and oxygen are also applicable.
- gases such as nitrogen and oxygen are also applicable.
- the formation of anisotropic particles starts from a high temperature, intragranularity that impedes translucency by advancing densification with fine sintered particles in atmospheric pressure sintering. Densification proceeds without generating pores. Further, in the subsequent HIP treatment, the growth of anisotropic particles characteristic of the sintered body of the present invention is promoted, high translucency is maintained, and a highly aesthetic colored and high toughness alumina sintered body is obtained. .
- Fracture toughness The fracture toughness test was measured by the SEPB method based on JIS R1607 “Fracture toughness test method for fine ceramics”. An average value of 5 was adopted.
- Bending strength The bending test was measured by a three-point bending test based on JIS R1601 “Bending strength test method of fine ceramics”, and an average value of 10 pieces was adopted.
- the total light transmittance is based on JISK7105 “Testing method for optical properties of plastics” and JISK7361-1 “Testing method for total light transmittance of plastics and transparent materials”. (Measured by JASCO Corporation, model V-650).
- the light emitted from the light source deuterium lamp and halogen lamp
- the measurement wavelength region was measured in the region of 200 to 800 nm, and the total light transmittance in this case was the maximum value at a wavelength of 300 to 800 nm.
- the chemical etching was performed by a method in which the sintered body was immersed in a supersaturated sodium borate solution at 80 ° C. and adhered to the surface, heated at 900 ° C. for 0.5 hours, cooled, and then washed with a hydrochloric acid solution.
- Density of sintered body The density was determined by Archimedes method for measuring the weight of the sintered body in water. The relative density was calculated with a theoretical density of 3.98 g / cm 3 .
- Example 1 High purity alumina powder ( ⁇ -Al 2 O 3 : manufactured by Daimei Chemical Industries, purity 99.99% or more), manganese oxide (MnO: high purity chemical, purity 99.9%), nickel oxide (NiO: rare metal, Purity 99.99%), copper oxide (CuO: Wako Pure Chemical, purity 99.9%), vanadium oxide (V 2 O 5 : Wako Pure Chemical primary reagent), iron oxide (Fe 3 O 4 , Kanto Chemical, first grade) Reagent) and titanium oxide (TiO 2 : Kishida Chemical, purity 99.5%) were added, and ball mill mixed in ethanol and dried to obtain a raw material powder. The amount of transition metal oxide added was 500 ppm with respect to alumina. Table 1 shows impurities contained in the high-purity alumina powder used as a raw material. The total amount of these was 20 ppm or less. In addition, about what was not described in Table 1, it was below the detection limit ( ⁇ 1 ppm).
- the powder having the composition shown in Table 2 is applied to a plate-shaped product of 40 mm ⁇ 50 mm and 5 mm thickness by applying a pressure of 50 MPa, and this is put in a rubber mold and a pressure of 200 MPa using a cold isostatic press device. And hardened. These were sintered in the atmosphere at 1300 ° C. for 2 hours to obtain a primary sintered body.
- the primary sintered body was treated with an HIP apparatus in an argon gas medium at a temperature of 1450 to 1650 ° C. and a pressure of 150 MPa for 1 hour.
- the sintered body thus obtained was measured for the proportion of anisotropic particles having a major axis length of 10 ⁇ m or more and an aspect ratio of 1.5 or more, fracture toughness, bending strength, and total light transmittance. The results are shown in Table 2. It was revealed that a colored translucent alumina sintered body having both high fracture toughness and high translucency can be obtained.
- Example 2 To the high-purity alumina powder described in Example 1, cobalt oxide (CoO: manufactured by Rare Metallic, purity 99.9%), chromium oxide (Cr 2 O 3 : Rare Metallic, purity 99.99%), manganese oxide, vanadium oxide Nickel oxide and sodium metasilicate (Na 2 O ⁇ SiO 2 , manufactured by ALDRICH) were added, ball milled in ethanol, and dried to obtain a raw material powder. The addition amounts of transition metal oxide and sodium metasilicate were 500 ppm and 50 ppm, respectively, with respect to alumina.
- a sintered body was obtained by the same treatment as in Example 1 except that the powder having the composition shown in Table 3 was used.
- the sintered body thus obtained was measured for the proportion of anisotropic particles having a major axis length of 10 ⁇ m or more and an aspect ratio of 1.5 or more, fracture toughness, bending strength, and total light transmittance.
- the results are shown in Table 3. It was revealed that a colored translucent alumina sintered body having both high fracture toughness and high translucency can be obtained.
- Comparative Example 1 Using the high-purity alumina powder described in Example 1, a sintered body was produced under the same conditions as in Example 1 for chromium oxide and cobalt oxide having no eutectic point with alumina. Table 4 shows the results of coloring, fracture toughness, bending strength, and total light transmittance (maximum value at a sample thickness of 1 mm and a wavelength of 300 to 800 nm) of the sintered body. In a sintered body containing only a transition metal oxide having no eutectic point with alumina, anisotropic particles did not grow, and only a low toughness sintered body was obtained.
- the colored translucent alumina sintered body of the present invention has both high toughness and translucency, and is used not only for conventional ornaments, jewelry and crafts, but also as a high toughness value and fashion that does not break during processing. It is suitable for dental materials such as orthodontic brackets and dental restoration mill blanks that require coloring aesthetics. Therefore, the industrial value of the present invention is remarkable.
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Abstract
La dureté à la cassure et la translucidité de l'alumine transparente colorée frittée du passé étant faibles, l'alumine n'était pas adaptée pour des utilisations telles que des matériaux dentaires, qui requièrent une dureté élevée. L'invention concerne une alumine translucide colorée frittée qui renferme un oxyde de métaux de transition, et avec laquelle la dureté à la cassure est supérieure à 4,5 MPa m0,5 et la valeur maximale de la transmittance totale (échantillon d'une épaisseur d'1 mm), par rapport aux longueurs d'onde de 300 à 800 nm, est de 60 % ou plus. L'invention concerne une alumine frittée renfermant un oxyde de métaux de transition présentant un point eutectique avec l'alumine, ou une alumine frittée renfermant un oxyde de métaux de transition et au moins un élément choisi dans le groupe constitué des oxydes de métaux alcalins de groupe 1A, les oxydes de métaux terreux alcalins de groupe 2A et SiO2, B2O3, P2O5 et GeO2, est frittée et traitée par CIC à une pression normale pour obtenir un corps fritté, au moins 20 % de celui-ci renfermant des particules anisotropes avec un axe principal d'une longueur de 10 µm ou supérieure et un rapport de forme de 1,5 ou plus.
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US13/121,884 US8481439B2 (en) | 2008-11-18 | 2009-11-13 | Colored alumina sintered body of high toughness and high translucency, and its production method and its uses |
EP09827526.6A EP2366675B1 (fr) | 2008-11-18 | 2009-11-13 | Alumine colorée frittée de dureté et translucidité élevées, et procédé de fabrication et ses utilisations |
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JP2008294499A JP5458553B2 (ja) | 2008-11-18 | 2008-11-18 | 高靭性且つ透光性の着色アルミナ焼結体及びその製造方法並びに用途 |
JP2008294498A JP5458552B2 (ja) | 2008-11-18 | 2008-11-18 | 高靭性且つ透光性の着色アルミナ焼結体及びその製造方法並びに用途 |
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JP2019084824A (ja) * | 2017-11-08 | 2019-06-06 | キヤノン株式会社 | セラミックス造形用粉体およびそれを用いたセラミックスの造形方法 |
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RU2494994C1 (ru) * | 2012-04-11 | 2013-10-10 | Федеральное Государственное Автономное Образовательное Учреждение Высшего Профессионального Образования "Сибирский Федеральный Университет" | Способ получения корундовой керамики |
WO2014096142A1 (fr) * | 2012-12-19 | 2014-06-26 | Ceramtec-Etec Gmbh | Matériau céramique |
US9527774B2 (en) * | 2014-08-27 | 2016-12-27 | King Abdulaziz City For Science And Technology | High strength transparent ceramic using corundum powder and methods of manufacture |
US9287106B1 (en) | 2014-11-10 | 2016-03-15 | Corning Incorporated | Translucent alumina filaments and tape cast methods for making |
RU2676309C1 (ru) * | 2017-09-11 | 2018-12-27 | Федеральное Государственное Бюджетное Образовательное Учреждение Высшего Образования "Новосибирский Государственный Технический Университет" | Корундовая керамика и способ ее получения |
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JP2019084824A (ja) * | 2017-11-08 | 2019-06-06 | キヤノン株式会社 | セラミックス造形用粉体およびそれを用いたセラミックスの造形方法 |
JP7256630B2 (ja) | 2017-11-08 | 2023-04-12 | キヤノン株式会社 | セラミックス造形用粉体およびそれを用いたセラミックスの造形方法 |
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EP2366675A1 (fr) | 2011-09-21 |
EP2808313A3 (fr) | 2015-02-25 |
US8481439B2 (en) | 2013-07-09 |
US20110189622A1 (en) | 2011-08-04 |
EP2808313A2 (fr) | 2014-12-03 |
EP2366675A4 (fr) | 2013-04-24 |
EP2366675B1 (fr) | 2015-05-27 |
EP2808313B1 (fr) | 2018-05-02 |
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