CN108329036B - 一种超细高纯AlON粉体及其制备方法 - Google Patents

一种超细高纯AlON粉体及其制备方法 Download PDF

Info

Publication number
CN108329036B
CN108329036B CN201810148003.8A CN201810148003A CN108329036B CN 108329036 B CN108329036 B CN 108329036B CN 201810148003 A CN201810148003 A CN 201810148003A CN 108329036 B CN108329036 B CN 108329036B
Authority
CN
China
Prior art keywords
powder
purity
alon
preparation
mixed
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.)
Active
Application number
CN201810148003.8A
Other languages
English (en)
Other versions
CN108329036A (zh
Inventor
李庆刚
王志
史国普
黄世峰
程新
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
University of Jinan
Original Assignee
University of Jinan
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by University of Jinan filed Critical University of Jinan
Priority to CN201810148003.8A priority Critical patent/CN108329036B/zh
Publication of CN108329036A publication Critical patent/CN108329036A/zh
Application granted granted Critical
Publication of CN108329036B publication Critical patent/CN108329036B/zh
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

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
    • C04B35/515—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
    • 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
    • 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
    • C04B35/62615—High energy or reactive ball 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
    • C04B35/62625—Wet mixtures
    • C04B35/6264—Mixing media, e.g. organic solvents
    • 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
    • C04B35/64—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
    • 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
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
    • 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
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/422—Carbon
    • 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
    • C04B2235/5454—Particle size related information expressed by the size of the particles or aggregates thereof nanometer sized, i.e. below 100 nm
    • 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
    • C04B2235/658—Atmosphere during thermal treatment
    • C04B2235/6586—Processes characterised by the flow of gas
    • 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
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Structural Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Ceramic Products (AREA)

Abstract

本发明涉及一种超细高纯AlON粉体及其制备方法，属于透明陶瓷粉体制备领域。该方法通过以下步骤实现：首先制备Al2O3和碳粉的混合粉体；然后将混合粉体至于BN坩埚中，采用气氛压力烧结制备得超细高纯AlON粉体。本发明采用传统氧化铝和碳粉为原材料，在相对低温的条件下制备出AlON粉体，制备工艺简单可控，可操作性强；本发明制备的AlON粉体纯度较高，粒度较小。

Description

一种超细高纯AlON粉体及其制备方法
技术领域
本发明涉及一种超细高纯AlON粉体及其制备方法，属于透明陶瓷粉体制备领域。
背景技术
红外窗口是结构功能一体化的重要部件，在导弹光电系统中起着重要的作用，但随着科学技术的不断发展，对其性能提出了更高的要求。目前普遍公认的三种最有潜力的红外窗口材料是蓝宝石、多晶镁铝尖晶石、多晶氧氮化铝(AlON)，他们各有优缺点，但就综合性能而言，AlON透明陶瓷是最具竞争力的红外窗口材料。
透明氮氧化铝 (γ- AlON) 是A12O3-AlN二元系中一个单相、稳定的固溶体透明陶瓷，它不仅具有优良的物理、力学、化学性质，而且具有良好的光学透过性
尤其是从紫外到中红外波段(0.2-5.0 μm)的透光率高达80%，因此被广泛地运用到军事和商业等领域。目前AlON透明陶瓷已成为高温红外窗、防弹装甲材料和双模天线罩的优先候选材料之一。AlON陶瓷通常采用两步法制备，即首先合成AlON粉体，然后进行成型和烧结，其中，AlON粉体的制备是研制AlON透明陶瓷的关键技之一。AlON粉体的晶体结构与缺陷、分散性、纯度与粒度均会影响AlON透明陶瓷的透明度。但是制备的AlON粉体往往会发生团聚，粉体的粒度较大，这会导致在一定的成型密度下，颗粒之间的气孔较大，烧结时空穴的扩散不容易进行，不利于气孔的排除，制备的陶瓷透明度不理想。而且传统方法制备AlON粉体温度较高，不利于AlON透明陶瓷成本的控制。因此，研究探索低温制备AlON粉体粒度的方法具有非常重要的意义。
发明内容
本发明的目的在于提供一种超细高纯AlON粉体的制备方法，在相对低温的条件下，得到纯度较高、粒度较小的AlON粉体。
本发明还提供了一种利用上述制备方法制备的超细高纯AlON粉体。
本发明为了实现上述目的所采用的技术方案为：
本发明提供了一种超细高纯AlON粉体的制备方法，其特征在于，包括以下步骤：
（1）制备Al2O3和碳粉的混合粉体：将Al2O3粉末、碳粉和无水乙醇混合，在室温下进行磁力搅拌及超声分散20min得到混合浆料；随后将混合浆料放入聚四氟乙烯罐中进行行星式球磨12小时，球磨介质为氧化锆球；球磨后的浆料干燥得混合粉体；然后经过研磨后过200目筛备用；
（2）AlON粉体的低温制备技术：将混合粉体至于BN坩埚中，采用气氛压力烧结制备得超细高纯AlON粉体。
进一步的，所述碳粉在混合浆料中的质量分数为5.4-7.0wt%；所述Al2O3粉末和无水乙醇的质量比为1：20。
进一步的，所述球磨的球料比1：10；转速为200rpm。
进一步的，步骤（1）中，所述干燥为在真空干燥箱中，80℃下干燥4h。
进一步的，所述气氛压力烧结为分段进行，首先，得到的混合粉体在流动高纯氮气气氛保护条件下以10℃/min升温至1450-1550℃并保温1-2h；然后，以3℃/min升温至1650-1800℃并保温2-4h，气氛压力为0.1-4MPa；最后在马弗炉中700℃条件下保温4h，得到高纯的AlON粉体。
本发明还提供了一种上述制备方法制备的超细高纯AlON粉体，该粉体的纯度为95.62-99.63%；粒度小于100nm。
本发明的有益效果为：
（1）本发明采用传统氧化铝和碳粉为原材料，在相对低温的条件下制备出AlON粉体，制备工艺简单可控，可操作性强；
（2）本发明制备的AlON粉体纯度较高，粒度较小。
附图说明
图1为实施例中不同温度下制备的AlON粉体的XRD图谱。
图2为实施例中AlON粉体的SEM照片。
图3为实施例中AlON粉体的颜色。
具体实施方式
下面以具体的实施例对本发明的技术方案作进一步的解释和说明。
实施例1
将氧化铝粉末、碳粉和无水乙醇按照一定的质量比进行混合，其中碳粉在混合浆料中的含量控制在5.4wt%，Al2O3粉末和无水乙醇的质量比为1：20，在室温下进行磁力搅拌及超声分散20min得到混合浆料；随后将混合浆料放入聚四氟乙烯罐中进行行星式球磨12小时，球磨介质为氧化铝球；球磨后的浆料放入真空干燥箱中在80℃下干燥2h得混合粉体；然后经过研磨后过200目筛备用；称取一定质量的混合粉末，在流动氮气气氛中进行高温处理。烧结工艺为气氛压力烧结：分两步完成。首先，得到的混合粉体在流动高纯氮气气氛保护条件下以10℃/min升温至1450℃并保温2h，得到AlN粉体；然后，以3℃/min升温至1650℃并保温2h，得到AlON粉体；气氛压力为0.1-4MPa；最后在马弗炉中700℃条件下保温4h对AlON粉体进行提纯，得到高纯的AlON粉体。该实施例制备的粉体的纯度为99.63%；粒度小于100nm。
实施例2
将氧化铝粉末、碳粉和无水乙醇按照一定的质量比进行混合，其中碳粉在混合浆料中的含量控制在6wt%，Al2O3粉末和无水乙醇的质量比为1：20，在室温下进行磁力搅拌及超声分散20min得到混合浆料；随后将混合浆料放入聚四氟乙烯罐中进行行星式球磨12小时，球磨介质为氧化铝球；球磨后的浆料放入真空干燥箱中在80℃下干燥2h得混合粉体；然后经过研磨后过200目筛备用；称取一定质量的混合粉末，在流动氮气气氛中进行高温处理。烧结工艺为气氛压力烧结：分两步完成。首先，得到的混合粉体在流动高纯氮气气氛保护条件下以10℃/min升温至1450℃并保温1-2h，得到AlN粉体；然后，以3℃/min升温至1700℃并保温3h，得到AlON粉体；气氛压力为0.1-4MPa；最后在马弗炉中700℃条件下保温4h对AlON粉体进行提纯，得到高纯的AlON粉体。该实施例制备的粉体的纯度为98.82%；粒度小于100nm。
实施例3
将氧化铝粉末、碳粉和无水乙醇按照一定的质量比进行混合，其中碳粉在混合浆料中的含量控制在6.5wt%，Al2O3粉末和无水乙醇的质量比为1：20，在室温下进行磁力搅拌及超声分散20min得到混合浆料；随后将混合浆料放入聚四氟乙烯罐中进行行星式球磨12小时，球磨介质为氧化铝球；球磨后的浆料放入真空干燥箱中在80℃下干燥2h得混合粉体；然后经过研磨后过200目筛备用；称取一定质量的混合粉末，在流动氮气气氛中进行高温处理。烧结工艺为气氛压力烧结：分两步完成。首先，得到的混合粉体在流动高纯氮气气氛保护条件下以10℃/min升温至1550℃并保温1h，得到AlN粉体；然后，以3℃/min升温至1750℃并保温2h，得到AlON粉体；气氛压力为0.1-4MPa；最后在马弗炉中700℃条件下保温4h对AlON粉体进行提纯，得到高纯的AlON粉体。该实施例制备的粉体的纯度为99.11%；粒度小于100nm。
实施例4
将氧化铝粉末、碳粉和无水乙醇按照一定的质量比进行混合，其中碳粉在混合浆料中的含量控制在7wt%，Al2O3粉末和无水乙醇的质量比为1：20，在室温下进行磁力搅拌及超声分散20min得到混合浆料；随后将混合浆料放入聚四氟乙烯罐中进行行星式球磨12小时，球磨介质为氧化铝球；球磨后的浆料放入真空干燥箱中在80℃下干燥2h得混合粉体；然后经过研磨后过200目筛备用；称取一定质量的混合粉末，在流动氮气气氛中进行高温处理。烧结工艺为气氛压力烧结：分两步完成。首先，得到的混合粉体在流动高纯氮气气氛保护条件下以10℃/min升温至1550℃并保温1h，得到AlN粉体；然后，以3℃/min升温至1800℃并保温2h，得到AlON粉体；气氛压力为0.1-4MPa；最后在马弗炉中700℃条件下保温4h对AlON粉体进行提纯，得到高纯的AlON粉体。该实施例制备的粉体的纯度为95.62%；粒度小于100nm。
图1为实施例1-4不同温度下制备的AlON粉体的XRD图谱，在较低温度下可以得到纯度较高的AlON粉体。图2为不同温度下得到的AlON粉体的SEM照片，在较低的温度下能得到粒度小的AlON粉末；图3为不同温度下得到的AlON粉体的颜色，比较得出在较低的温度下可以得到白色的AlON粉体，有利于制备AlON透明陶瓷。

Claims (5)

1.一种超细高纯AlON粉体的制备方法，其特征在于，包括以下步骤：
（1）制备Al2O3和碳粉的混合粉体：将Al2O3粉末、碳粉和无水乙醇混合，在室温下进行磁力搅拌及超声分散20min得到混合浆料；随后将混合浆料放入聚四氟乙烯罐中进行行星式球磨12小时，球磨介质为氧化锆球；球磨后的浆料干燥得混合粉体；然后经过研磨后过200目筛备用；
（2）AlON粉体的低温制备技术：将混合粉体至于BN坩埚中，采用气氛压力烧结制备得超细高纯AlON粉体；
所述气氛压力烧结为分段进行，首先，得到的混合粉体在流动高纯氮气气氛保护条件下以10℃/min升温至1450-1550℃并保温1-2h；然后，以3℃/min升温至1650-1800℃并保温2-4h，气氛压力为0.1-4MPa；最后在马弗炉中700℃条件下保温4h，得到高纯的AlON粉体。
2.根据权利要求1所述的制备方法，其特征在于，所述碳粉在混合浆料中的质量分数为5.4-7.0wt%；所述Al2O3粉末和无水乙醇的质量比为1：20。
3.根据权利要求1或2所述的制备方法，其特征在于，所述球磨的球料比1：10；转速为200rpm。
4.根据权利要求1所述的制备方法，其特征在于，步骤（1）中，所述干燥为在真空干燥箱中，80℃下干燥4h。
5.一种采用如权利要求1-4任一项所述的制备方法制备的超细高纯AlON粉体，其特征在于，该粉体的纯度为95.62-99.63%；粒度小于100nm。
CN201810148003.8A 2018-02-13 2018-02-13 一种超细高纯AlON粉体及其制备方法 Active CN108329036B (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810148003.8A CN108329036B (zh) 2018-02-13 2018-02-13 一种超细高纯AlON粉体及其制备方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810148003.8A CN108329036B (zh) 2018-02-13 2018-02-13 一种超细高纯AlON粉体及其制备方法

Publications (2)

Publication Number Publication Date
CN108329036A CN108329036A (zh) 2018-07-27
CN108329036B true CN108329036B (zh) 2021-01-22

Family

ID=62929605

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810148003.8A Active CN108329036B (zh) 2018-02-13 2018-02-13 一种超细高纯AlON粉体及其制备方法

Country Status (1)

Country Link
CN (1) CN108329036B (zh)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111762765B (zh) * 2020-06-28 2023-05-09 中国科学院上海硅酸盐研究所 一种AlON粉体及其制备方法
CN112110424B (zh) * 2020-09-23 2022-04-12 航天特种材料及工艺技术研究所 一种超细氮化铝粉体的制备方法
CN116768634B (zh) * 2023-06-21 2024-04-09 成都光明光电有限责任公司 AlON粉体的抗水化方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02137711A (ja) * 1988-11-15 1990-05-28 Sumitomo Electric Ind Ltd 酸窒化アルミニウム粉末の製造方法
CN102557087A (zh) * 2011-12-16 2012-07-11 中国科学院上海硅酸盐研究所 一种制备高纯AlON粉体的方法
CN102731109A (zh) * 2012-06-16 2012-10-17 山东科技大学 一种AlON材料的合成方法
CN102807370A (zh) * 2012-08-15 2012-12-05 中国科学院宁波材料技术与工程研究所 一种碳热还原快速制备AlON陶瓷粉末的方法
CN105622104A (zh) * 2014-10-27 2016-06-01 天津津航技术物理研究所 一种高纯AlON透明陶瓷粉体的制备方法

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6955798B2 (en) * 2002-05-01 2005-10-18 Nanomat, Inc. Method for manufacturing aluminum oxynitride (AlON) powder and other nitrogen-containing powders

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02137711A (ja) * 1988-11-15 1990-05-28 Sumitomo Electric Ind Ltd 酸窒化アルミニウム粉末の製造方法
CN102557087A (zh) * 2011-12-16 2012-07-11 中国科学院上海硅酸盐研究所 一种制备高纯AlON粉体的方法
CN102731109A (zh) * 2012-06-16 2012-10-17 山东科技大学 一种AlON材料的合成方法
CN102807370A (zh) * 2012-08-15 2012-12-05 中国科学院宁波材料技术与工程研究所 一种碳热还原快速制备AlON陶瓷粉末的方法
CN105622104A (zh) * 2014-10-27 2016-06-01 天津津航技术物理研究所 一种高纯AlON透明陶瓷粉体的制备方法

Also Published As

Publication number Publication date
CN108329036A (zh) 2018-07-27

Similar Documents

Publication Publication Date Title
CN108329036B (zh) 一种超细高纯AlON粉体及其制备方法
CN107352994B (zh) 一种镁铝尖晶石透明陶瓷的制备方法
CN109400123B (zh) 一种细晶氧化铝陶瓷及其制备方法和应用
CN109369183B (zh) 一种红外透明陶瓷材料及其制备方法
CN108383530B (zh) 一种ZrB2-SiC陶瓷复合粉体的前驱体转化法制备工艺
CN101928145A (zh) 一种超细、高纯γ-AlON透明陶瓷粉末的制备方法
CN100387548C (zh) 增韧镁铝尖晶石透明陶瓷的制备方法
CN108640672A (zh) 一种镁铝尖晶石透明陶瓷的制备方法
CN103011827A (zh) 一种原位引入硼为添加剂的二硼化锆陶瓷的制备方法
CN109553419A (zh) 一种气压固相烧结碳化硼复相陶瓷及其制备方法
CN110272282B (zh) AlON透明陶瓷的低温制备方法
CN112299861B (zh) 一种AlON透明陶瓷伪烧结剂与应用及透明陶瓷的制备方法
CN114105639A (zh) 一种红外透明陶瓷材料及其制备方法
CN113149652A (zh) 基于冷烧结技术制备的高透光率透明陶瓷及其制备方法
CN104387081A (zh) 透明氮氧化铝(AlON)陶瓷的低温制备方法
Chen et al. Highly oriented α-Al2O3 transparent ceramics shaped by shear force
CN103755353B (zh) 一种Y-α-SiAlON透明陶瓷的快速低温制备方法
JP6450425B1 (ja) 球状酸窒化アルミニウム粉末の製造方法
CN113582696A (zh) 一种(ZrTiCoNb)C高熵碳化物陶瓷材料及其制备方法
CN109053192B (zh) 一种MgAlON透明陶瓷粉体的制备方法
CN116161966B (zh) 单相AlON粉体的制备方法
CN104016668A (zh) 一种莫来石陶瓷粉体的制备方法
CN115196969B (zh) 一种高红外透过率MgAlON透明陶瓷的固相反应快速无压烧结方法
CN109354501B (zh) 一种MgAlON透明陶瓷的制备方法
CN109437916A (zh) 高透明LiAlON陶瓷的制备方法

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant