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 PDF

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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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PCT/JP2009/069393
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English (en)
Japanese (ja)
Inventor
勲 山下
津久間　孝次
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東ソー株式会社
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Publication date
Priority claimed from JP2008294499A external-priority patent/JP5458553B2/ja
Priority claimed from JP2008294498A external-priority patent/JP5458552B2/ja
Application filed by 東ソー株式会社 filed Critical 東ソー株式会社
Priority to EP09827526.6A priority Critical patent/EP2366675B1/fr
Priority to US13/121,884 priority patent/US8481439B2/en
Publication of WO2010058745A1 publication Critical patent/WO2010058745A1/fr

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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • 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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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.

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.
PCT/JP2009/069393 2008-11-18 2009-11-13 Alumine colorée frittée de dureté et translucidité élevées, et procédé de fabrication et ses utilisations WO2010058745A1 (fr)

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US20110189622A1 (en) 2011-08-04
EP2808313A2 (fr) 2014-12-03
US8481439B2 (en) 2013-07-09
EP2366675B1 (fr) 2015-05-27
EP2366675A4 (fr) 2013-04-24
EP2366675A1 (fr) 2011-09-21
EP2808313A3 (fr) 2015-02-25

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