CN104220397A - 借助流化床造粒制备透明陶瓷物品的方法 - Google Patents
借助流化床造粒制备透明陶瓷物品的方法 Download PDFInfo
- Publication number
- CN104220397A CN104220397A CN201280066625.7A CN201280066625A CN104220397A CN 104220397 A CN104220397 A CN 104220397A CN 201280066625 A CN201280066625 A CN 201280066625A CN 104220397 A CN104220397 A CN 104220397A
- Authority
- CN
- China
- Prior art keywords
- pellet
- ceramic powder
- fluidized bed
- crystalline ceramics
- sintered compact
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/111—Fine ceramics
- C04B35/115—Translucent or transparent products
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/16—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by suspending the powder material in a gas, e.g. in fluidised beds or as a falling curtain
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/44—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 aluminates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/44—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 aluminates
- C04B35/443—Magnesium aluminate spinel
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—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
- 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
- C04B35/581—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 aluminium nitride
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/6261—Milling
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/62655—Drying, e.g. freeze-drying, spray-drying, microwave or supercritical drying
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/62695—Granulation or pelletising
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/6455—Hot isostatic pressing
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5427—Particle size related information expressed by the size of the particles or aggregates thereof millimeter or submillimeter sized, i.e. larger than 0,1 mm
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5445—Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/604—Pressing at temperatures other than sintering temperatures
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/608—Green bodies or pre-forms with well-defined density
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/661—Multi-step sintering
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/76—Crystal structural characteristics, e.g. symmetry
- C04B2235/762—Cubic symmetry, e.g. beta-SiC
- C04B2235/764—Garnet structure A3B2(CO4)3
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9646—Optical properties
- C04B2235/9653—Translucent or transparent ceramics other than alumina
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
本发明涉及一种在波长范围为300nm至4000nm,陶瓷壁厚度为2mm的条件下,具有>10%的RIT的透明陶瓷物品的生产方法。所述方法包括如下步骤:通过散布陶瓷粉末制作一种浆料,所述陶瓷粉末的粒料尺寸为d50<50μm,优选为5μm至500μm;通过流化床造粒,从上述浆料生产一种粒状材料,其粒径为d50<1mm,优选为50μm至500μm,更优选为80μm至300μm;将粒状材料以简单非循环的方式压制成坯体;烧结坯体制成烧结体;重致密化烧结体。
Description
本发明涉及透明陶瓷物品的生产方法,所述透明陶瓷物品在300nm至4000nm之间的波长范围在所述陶瓷物品的壁厚为2mm的情况下具有>10%的RIT。
这种陶瓷物品例如可用于弹道学中,因为其可在高硬度的同时实现所希望的透明度。另外的应用可能性例如在光学领域。
背景技术
为了保护车辆如军用车辆或民用车辆免受射击,通常给它们装甲。装甲大都借助金属-体系或借助金属-陶瓷-体系进行。然而,这样的已知体系不适用于汽车的侧窗玻璃、挡风玻璃等区域。给这些区域通常配备防弹玻璃。但是,防弹玻璃尤其对穿甲武器具有相对低的弹道学效率,所以窗户区域是这样配备的车辆的薄弱处。此外,防弹玻璃造成大的重量,以确保足够的防护。
透明陶瓷具有更好的防护性能,因此寻求防弹玻璃的替代品。这些替代品基本上在尖晶石和氮氧化铝(AlON)中找到。然而,由于需要很高的加工温度,这些已知材料是粗晶的,具有明显>1μm,或者甚至明显>10μm的粒径。这些已知替代品的另一不足之处在于其成本高昂,因为在一个持续数小时的制造周期中,仅能实现一小部分。由此导致如此生产的透明陶瓷物品需要数倍于防弹玻璃的成本。尽管已知的透明陶瓷物品拥有更好的特性,但它们迄今还未能在市场上占有显著的地位,或者其迄今只能进行实验室规模的生产。
因此,迫切希望一种更为经济的透明陶瓷物品的生产方法。此外,相较于迄今使用的粗晶热压材料,也希望改善结构特性。这种结构特性的改善例如描述于EP1557402A2通过凝胶浇铸。凝胶浇铸是湿法成型。除凝胶浇铸外,也已知注浆成型、压铸和电泳沉积(EPD)。然而所有这些已知方法均需要复杂的干燥及/或脱脂。此外,因为此种方式生产的陶瓷物品的表面品质还有许多待改进之处,所以需要进行复杂的表面后处理。
所以,希望寻求一种不复杂的经济的透明陶瓷物品的生产工艺。在经济性方面压制法尤其适合。然而,迄今没有任何具有所需光学和机械特性的陶瓷能用这种技术经济地生产。其原因尤其在于坯体烧结能力太低,该能力基本上由孔分布和孔体积决定。因为,在传统压制成型中,孔体积和尤其是孔分布比湿法成型方法差。
除了压制之外,造粒对于透明陶瓷物品的生产也十分重要。只有在存在最佳粒料时才能制备无缺陷材料。
大多数情况下使用的粒料是喷雾粒料。因其生产方式,喷雾粒料的孔比例较高,而且由于粒料的外壳暴露在比粒料中心明显更高的生产温度下,该粒料具有不规则结构。此外,总是发生水由粒料内部向外的扩散,所以在各颗粒内有梯度密度曲线。在大多数情况下,在粒料内甚至产生在压制粒料时不能完全均匀的空心区域。
Kim D.J.,Jung J.-Y″Granule performance of zirconia/alumina compositepowders spray-dried using polyvinyl pyrrolidone binder,",J.E.Ceram Soc.27(2007)3177-3182描述了基于喷雾造粒的实心粒料;但其仍然存在在粒料的边缘区域与中心区域之间的暴露温度不同的问题。这将导致较宽的孔分布。
为回避上述问题的一种可能性是冷冻造粒;它产生非常均质且均匀结构的粒料,因此在烧结的陶瓷中产生好的性能。然而,迄今在陶瓷领域此技术仅以实验室规模应用,且不适用于大规模生产。此技术使用液氮进行生产,需要很高的制造成本。在喷雾之后,该材料还必须在另一步骤中冷冻干燥。
由申请人的DE 10 2007 059 091 Al中已知一种制备在600nm至650nm之间的相对小的光波长范围内具有RIT>40%的透明陶瓷的方法。作为关键工艺步骤,此方法利用粒料的循环压制来制作胚体。在这种已知方法中,可将通过喷雾造粒、通过冷冻造粒或通过流化床造粒制备的常规陶瓷颗粒通过循环压制制成在上述波长范围内透明的陶瓷物品。
本发明的目的是实现本文开始提及类型的方法,由此用已知的工艺技术通过特殊陶瓷粒料的单轴压制或冷等静压成型可以制备在宽的波长范围内透明的陶瓷物品。
根据本发明,上述目的通过权利要求1的特征得以实现。本发明所述方法的优选实施方案和/或扩展方案在从属权利要求中表明。
根据本发明生产的陶瓷物品例如在600nm-700nm、1000nm-1400nm和2000nm-2400nm之间的波长范围内,在壁厚度为2mm的情况下,具有>10%的RIT。即意外地发现,通过已知的流化床造粒可以实现上述类型的透明陶瓷物品。在此,特别之处在于流化床粒料的特殊性质和这种特殊性质对透明陶瓷物品的生产的作用,不需要如在此前引用的DE 10 2007 059 091 Al中公开的粒料的循环压制用于制备相应的胚体。
本发明所述的方法也适用于以有利的方式生产具有弹道保护特性的透明陶瓷物品。此透明陶瓷物品例如是车窗或者红外-雷达天线整流罩等部件。
意外地发现,流化床造粒具有最优化潜力,这使其可以生产相应于以非常复杂并因此仅用实验室规模使用冷冻造粒工艺获得的品质的粒料。已意外地表明,用流化床造粒生产的粒料令人惊讶地具有改善的变形性能并带来更低的孔隙率。粒料的实心粒状结构及无梯度的结构是可能的,因为通过根据本发明的造粒方法在粒料的外壳和粒料内部之间不产生温度梯度。不仅所述实心粒料,而且此外由于所述连续结构造成的粒料的无梯度性均以有利的方式能够使得根据本发明通过流化床造粒制备的粒料特别适用于透明陶瓷物品。不取决于所使用的陶瓷粉末,根据本发明制备的粒料在透明陶瓷物品的胚体压制过程中表现出最佳性能;由此,与根据DE 10 2007 059 091 Al的循环压制相反,以有利的方式可以或实现了简单的非循环的粒料压制。此外,常见不透明陶瓷小于0.1%的小的残留孔隙率在其性能方面几乎没有带来优点。然而,在透明陶瓷的情况中,残留孔隙率却形成不透明性和透明性之间的差异。由此,根据本发明的生产工艺特别适用于生产透明陶瓷物品。
如下表和附图1所示,在不适用于透明陶瓷物品的常规粉末中,在较低的温度和密度下就已经可以看出这些一般的优点;曲线a表示参照喷雾粒料的相对烧结密度和温度之间的函数关系,曲线b表示根据本发明的流化床粒料的相应函数关系。
根据本发明,在相对较低的温度条件下已经可以达到>99%的密度。在参照喷雾粒料的情况中,在1600℃下也无法达到>99%的密度。
表
根据本发明可以减少孔分布的宽度并从而增加均匀性。尤其是大孔消失。如图1可知,根据本发明,致密烧结温度下降超过50℃。此外,可实现更高的整体致密化。这是透明陶瓷所必需的。根据本发明,可以以更优的方式,通过简单传统的非循环压制达到所需的均匀性。此外,流化床方法适用于没有困难地以例如多于2,000吨/年的装置中造粒,因此适用于大规模生产。
根据本发明获得使用的流化床方法以意外的方式最适用于通过简单地将通过流化床造粒产生的粒料非循环压制成坯体来生产透明陶瓷物品。流化床造粒作物唯一的方法通过简单的非循环压制解决了经济性和大规模生产适应性的问题,并产生所希望的材料特性。
随后将成型压制过的坯体烧结并后致密化(nachverdichtet)。为此,可将坯体预烧结和热等静压成型烧结(sintergehippt),或者烧结至闭孔孔隙率并随后进行后热等静压成型(Nachgehippt)。
为进行最终的制备,可将该烧结体经过打磨并抛光至期望的光学品质,由此获得>10%的RIT。
本发明包括所有借助本发明的方法生产的陶瓷物品。本发明生产的透明陶瓷物品的几何形状由胚体加工的可能性,如CNC-铣切、切割、车削等决定。
决定所制备的陶瓷物品的透光性(透明度)的量值是为从检测到的强度中排除散射光仅用非常窄的约0.5DEG的孔径角测量的“真实直线透过率(RIT)”,其例如用波长为640nm的光(红光)测定。
根据本发明生产的陶瓷物品由透明多晶陶瓷制成,所述多晶陶瓷几乎不含玻璃相(小于0.1%),且具有>99.5%,优选>99.9%的理论密度。
在根据本发明的方法中,可以使用所有硬度≥10GPa且在孔隙率≤0.1%的情况下透明的陶瓷材料。优选氧化铝、尖晶石(MgAl2O4等)、AION、钙钛矿(例如YAlO3)或石榴石(例如Y3Al5O12)。前提条件仅为起始材料具有≥99%的纯度,且起始粒径≤1000μm,优选≤300nm。该陶瓷应几乎不含孔隙率(≤0.1%)以确保RIT-值≥10%。这是与已知的通过压制成型制备的“半透明”陶瓷,例如EP 1 458 304Al中所述的“半透明”陶瓷的明显区别。
根据本发明通过流化床造粒制备的粒料通过干燥压制或通过等静压成型或两者的结合成型为各自所希望的坯体。随后进行烧结和后致密化。后致密化优选通过热等静压成型(HIP)进行。HIP-过程可以在多种烧结气氛如氩气中或空气中或者真空进行。
或者也可将坯体按常规预烧结,然后热等静压成型(HIP)。烧结温度和HIP-温度取决于所用原材料和成型。为了获得所希望的透明度,在预烧结的情况中,后热等静压成型必不可少;在烧结热等静压成型的情况中,整个烧结在HIP-炉中进行。
下面借助两个实施例对本发明进行进一步详述。
实施例1:
将尖晶石粉末加工成50质量%的浆料。随后,将该稀粘稠的浆料借助偏心螺杆泵喷洒到流化床造粒装置中。纯粉末已预先作为粉末床加入到该装置中。通过缓慢而连续的浆料供给使材料缓慢持续地造粒。如此调节压力比例和进气,以生产出尺寸在介于d10=100μm和d90=300μm之间的范围的粒料。如此生产的粒料是实心粒料,其绝不具有如空心球结构或者环形结构的不均匀性。随后将该粒料在160MPa下单轴压制成50mm×50mm尺寸的板,因其均匀性,其可以在1500℃下致密烧结。然后,同样在1500℃和2000巴下进行HIP-过程。在HIP-过程后,根据阿基米德定律类似于DINEN623-2测定得到密度为3.575g/cm3。这是>99.9%的密度。由于高度均匀的密度,在所制成的板材内产生83%的RIT-值,具有0.2%的波动。
实施例2:
用搅拌式球磨机研磨氧化铝粉末,并加入合适的添加剂进一步加工成60质量%的浆料。随后,将该稀粘稠的浆料借助偏心螺杆泵喷洒到流化床造粒装置中。纯粉末已预先作为粉末床加入到该装置中。通过缓慢而连续的浆料供给使材料缓慢持续地造粒。如此调节压力比例和进气,以生产出尺寸在介于d10=80μm和d90=250μm之间的范围的粒料。如此生产的粒料是实心粒料,其绝不具有如空心球结构或者环形结构的不均匀性。随后将制备的粒料在150MPa下单轴压制成50mm×50mm尺寸的板,因其均匀性,其可以在1230℃下致密烧结。然后,同样在1200℃和2000巴下进行HIP-过程。在HIP-过程后,得到经测量>3.98g/cm3的密度。这是>99.9%的密度。由于高度均匀的密度,在壁厚为0.8mm的情况下得到>40%的RIT-值。
Claims (7)
1.透明陶瓷物品的生产方法,所述透明陶瓷物品在300nm至4000nm的波长范围内,在所述陶瓷物品的壁厚为2mm的情况下,具有>10%的RIT,
其特征在于以下方法步骤:
通过分散陶瓷粉末生产浆料,所述陶瓷粉末具有d50<5μm,优选在5nm至500nm之间的粒径,
由上述浆料通过流化床造粒生产粒料,所述粒料具有d50<1mm,优选在50μm至500μm之间的,更优选在80μm至300μm之间的粒径,
将所述粒料简单地非循环压制成坯体,
将所述胚体烧结成烧结体,以及
后致密化所述烧结体。
2.根据权利要求1所述的方法,其特征在于,所述陶瓷粉末的分散用水和表面活性物质进行。
3.根据权利要求1所述的方法,其特征在于,在分散时研磨所述陶瓷粉末。
4.根据权利要求1-3任一项所述的方法,其特征在于,所述陶瓷粉末的分散及研磨在搅拌研磨机中进行。
5.根据权利要求1所述的方法,其特征在于,所述坯体通过单轴压制和/或冷等静压而成型。
6.根据权利要求1所述的方法,其特征在于,通过热等静压(HIP)进行所述后致密化。
7.根据权利要求1所述的方法,其特征在于,将所述烧结体打磨并抛光至光学品质。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102011086100 | 2011-11-10 | ||
DE102011086100.9 | 2011-11-10 | ||
PCT/EP2012/072344 WO2013068576A1 (de) | 2011-11-10 | 2012-11-12 | Verfahren zur herstellung transparenter keramikgegenstände mittels wirbelschichtgranulation |
Publications (1)
Publication Number | Publication Date |
---|---|
CN104220397A true CN104220397A (zh) | 2014-12-17 |
Family
ID=47143935
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201280066625.7A Pending CN104220397A (zh) | 2011-11-10 | 2012-11-12 | 借助流化床造粒制备透明陶瓷物品的方法 |
Country Status (11)
Country | Link |
---|---|
US (1) | US20140374931A1 (zh) |
EP (1) | EP2776378A1 (zh) |
JP (1) | JP2015501775A (zh) |
KR (1) | KR20140103938A (zh) |
CN (1) | CN104220397A (zh) |
BR (1) | BR112014011382A8 (zh) |
DE (1) | DE102012220518A1 (zh) |
IL (1) | IL232543A0 (zh) |
IN (1) | IN2014CN04217A (zh) |
RU (1) | RU2014123398A (zh) |
WO (1) | WO2013068576A1 (zh) |
Families Citing this family (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2016021346A1 (ja) * | 2014-08-08 | 2016-02-11 | 信越化学工業株式会社 | 透明セラミックスの製造方法 |
CN105732011A (zh) * | 2014-12-10 | 2016-07-06 | 辽宁利永盛新材料有限公司 | 一种新型多功能硅藻土陶粒的制备方法 |
WO2018174814A1 (en) * | 2017-03-23 | 2018-09-27 | Dso National Laboratories | A protective material |
CN109836089A (zh) * | 2017-11-27 | 2019-06-04 | 辽宁法库陶瓷工程技术研究中心 | 一种多功能免烧型呼吸砖的制备方法 |
CN112299828A (zh) * | 2020-11-09 | 2021-02-02 | 新沂市锡沂高新材料产业技术研究院有限公司 | 一种应用于5g太阳能手机的透明陶瓷背板的制备方法 |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2011012125A1 (de) * | 2009-07-30 | 2011-02-03 | Fraunhofer Gesellschaft Zur Förderung Der Angewandten Forschung E. V. | α-Al2O3-SINTERMATERIAL UND VERFAHREN ZUR HERSTELLUNG EINES HOCHDICHTEN UND FEINSTKRISTALLINEN FORMKÖRPERS AUS DIESEM MATERIAL SOWIE DEREN VERWENDUNG |
Family Cites Families (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4761390A (en) * | 1987-02-02 | 1988-08-02 | Raytheon Company | Optically transparent yttrium oxide |
JP2620287B2 (ja) * | 1988-03-09 | 1997-06-11 | 住友電気工業株式会社 | 透光性スピネル焼結体の製造方法 |
DD274980A1 (de) * | 1988-08-29 | 1990-01-10 | Leuna Werke Veb | Verfahren zur herstellung sphaerischer formlinge |
DE4304809A1 (de) * | 1993-02-17 | 1994-08-18 | Glatt Ingtech Gmbh | Verfahren zur Herstellung von feinkeramischem Preßgranulat mittels Wirbelschichtgranulationstrocknung |
DE19602525A1 (de) * | 1996-01-25 | 1997-08-07 | Starck H C Gmbh Co Kg | Sphärische Keramikformkörper, Verfahren zu ihrer Herstellung sowie deren Verwendung |
US6878456B2 (en) | 2001-12-28 | 2005-04-12 | 3M Innovative Properties Co. | Polycrystalline translucent alumina-based ceramic material, uses, and methods |
DE102004004259B3 (de) | 2004-01-23 | 2005-11-24 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Transparente polykristalline Sinterkeramik kubischer Kristallstruktur |
DE102007059091A1 (de) * | 2007-12-07 | 2009-06-10 | ETEC Gesellschaft für technische Keramik mbH | Verfahren zur Herstellung einer polykristallinen transparenten Keramik |
FR2954766B1 (fr) * | 2009-12-24 | 2015-04-24 | Saint Gobain Ct Recherches | Poudre de granules de ceramique |
EP2776379A1 (de) * | 2011-11-07 | 2014-09-17 | CeramTec-Etec GmbH | Transparente keramik |
DE102013226579A1 (de) * | 2012-12-19 | 2014-06-26 | Ceramtec-Etec Gmbh | Keramikwerkstoff |
-
2012
- 2012-11-12 JP JP2014540497A patent/JP2015501775A/ja active Pending
- 2012-11-12 WO PCT/EP2012/072344 patent/WO2013068576A1/de active Application Filing
- 2012-11-12 EP EP12783242.6A patent/EP2776378A1/de not_active Withdrawn
- 2012-11-12 KR KR1020147015766A patent/KR20140103938A/ko not_active Application Discontinuation
- 2012-11-12 CN CN201280066625.7A patent/CN104220397A/zh active Pending
- 2012-11-12 BR BR112014011382A patent/BR112014011382A8/pt not_active Application Discontinuation
- 2012-11-12 RU RU2014123398/03A patent/RU2014123398A/ru not_active Application Discontinuation
- 2012-11-12 US US14/357,472 patent/US20140374931A1/en not_active Abandoned
- 2012-11-12 DE DE102012220518A patent/DE102012220518A1/de not_active Withdrawn
-
2014
- 2014-05-11 IL IL232543A patent/IL232543A0/en unknown
- 2014-06-05 IN IN4217CHN2014 patent/IN2014CN04217A/en unknown
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2011012125A1 (de) * | 2009-07-30 | 2011-02-03 | Fraunhofer Gesellschaft Zur Förderung Der Angewandten Forschung E. V. | α-Al2O3-SINTERMATERIAL UND VERFAHREN ZUR HERSTELLUNG EINES HOCHDICHTEN UND FEINSTKRISTALLINEN FORMKÖRPERS AUS DIESEM MATERIAL SOWIE DEREN VERWENDUNG |
Also Published As
Publication number | Publication date |
---|---|
BR112014011382A8 (pt) | 2017-06-20 |
WO2013068576A1 (de) | 2013-05-16 |
RU2014123398A (ru) | 2015-12-20 |
IL232543A0 (en) | 2014-06-30 |
BR112014011382A2 (pt) | 2017-06-13 |
IN2014CN04217A (zh) | 2015-07-17 |
EP2776378A1 (de) | 2014-09-17 |
JP2015501775A (ja) | 2015-01-19 |
DE102012220518A1 (de) | 2013-05-16 |
US20140374931A1 (en) | 2014-12-25 |
KR20140103938A (ko) | 2014-08-27 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Carloni et al. | Transparent alumina ceramics fabricated by 3D printing and vacuum sintering | |
KR101502601B1 (ko) | 입방 구조를 가진 소결 제품 | |
Suárez et al. | Sintering to transparency of polycrystalline ceramic materials | |
Ghanizadeh et al. | Improved transparency and hardness in α-alumina ceramics fabricated by high-pressure SPS of nanopowders | |
CN104220397A (zh) | 借助流化床造粒制备透明陶瓷物品的方法 | |
Lallemant et al. | Transparent polycrystalline alumina obtained by SPS: Green bodies processing effect | |
CN103833370B (zh) | 一种复相陶瓷Si3N4-SiC的近尺寸制备方法 | |
KR20110020235A (ko) | 티탄산알루미늄계 세라믹스의 제조 방법 | |
KR102510257B1 (ko) | 투명 스피넬 소결체, 광학 부재 및 투명 스피넬 소결체의 제조 방법 | |
CN106810251A (zh) | 高纯高致密氧化锆3d陶瓷外壳的生产方法 | |
KR20110083634A (ko) | 티탄산알루미늄계 세라믹스의 제조 방법 | |
CN108794016B (zh) | 一种高红外透过率AlON透明陶瓷的快速制备方法 | |
KR20120057615A (ko) | 티탄산알루미늄계 세라믹스의 제조 방법 및 티탄산알루미늄계 세라믹스 | |
CN104909725B (zh) | 一种无指甲纹缺陷的氧化铝瓷球制备方法 | |
Alhaji et al. | Development of synthesis and granulation process of MgAl2O4 powder for the fabrication of transparent ceramic | |
KR20130112889A (ko) | 복합 산화물 소결체 및 그 제조방법, 스퍼터링 타겟 및 산화물 투명 도전막 및 그 제조방법 | |
KR102036300B1 (ko) | 기계적 강도가 향상된 마그네슘 알루미네이트 스피넬 투명세라믹 제조방법 및 마그네슘 알루미네이트 스피넬 투명세라믹 | |
CN103526295A (zh) | 高纯高硬度聚晶立方氮化硼块体材料及其制备方法 | |
CN115745607A (zh) | 一种红外透明陶瓷材料及其制备方法 | |
US20140364299A1 (en) | Transparent Polycrystalline Ceramic Material | |
JP3285620B2 (ja) | 透光性イットリウム−アルミニウム−ガーネット焼結体の製造方法 | |
CN100558673C (zh) | 等静压成型制备石英陶瓷的方法 | |
JPH03261648A (ja) | 多結晶アルミナ焼結体の製造方法 | |
Basiri et al. | Optimization of spray freeze drying parameters for spark plasma sintering of transparent MgAl2O4 spinel | |
Zhang et al. | Preparation of spherical AlON powder and high transparent ceramics by pressureless sintering |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20141217 |
|
RJ01 | Rejection of invention patent application after publication |