CN113735585B - 一种氧化铝/钛硅碳复合材料的制备方法 - Google Patents

一种氧化铝/钛硅碳复合材料的制备方法 Download PDF

Info

Publication number
CN113735585B
CN113735585B CN202110987687.2A CN202110987687A CN113735585B CN 113735585 B CN113735585 B CN 113735585B CN 202110987687 A CN202110987687 A CN 202110987687A CN 113735585 B CN113735585 B CN 113735585B
Authority
CN
China
Prior art keywords
composite material
titanium
carbon
alumina
silicon
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
CN202110987687.2A
Other languages
English (en)
Other versions
CN113735585A (zh
Inventor
李庆刚
张振宇
史国普
王志
孙孟勇
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 CN202110987687.2A priority Critical patent/CN113735585B/zh
Publication of CN113735585A publication Critical patent/CN113735585A/zh
Application granted granted Critical
Publication of CN113735585B publication Critical patent/CN113735585B/zh
Priority to US17/892,081 priority patent/US11673841B2/en
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
    • C04B35/56—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 carbides or oxycarbides
    • C04B35/565—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 carbides or oxycarbides based on silicon carbide
    • C04B35/575—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 carbides or oxycarbides based on silicon carbide obtained by 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
    • C04B35/515—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
    • C04B35/56—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 carbides or oxycarbides
    • C04B35/5607—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 carbides or oxycarbides based on refractory metal carbides
    • C04B35/5611—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 carbides or oxycarbides based on refractory metal carbides based on titanium carbides
    • C04B35/5615—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 carbides or oxycarbides based on refractory metal carbides based on titanium carbides based on titanium silicon carbides
    • 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
    • C04B35/117—Composites
    • 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
    • C04B35/628—Coating the powders or the macroscopic reinforcing agents
    • C04B35/62802—Powder coating materials
    • C04B35/62805—Oxide ceramics
    • C04B35/62813—Alumina or 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
    • C04B35/622—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
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
    • 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
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3817—Carbides
    • C04B2235/3826—Silicon carbides
    • 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
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3817—Carbides
    • C04B2235/3839—Refractory metal carbides
    • C04B2235/3843—Titanium carbides
    • 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
    • C04B2235/65—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
    • C04B2235/6562—Heating rate
    • 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
    • C04B2235/6567—Treatment time
    • 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
    • C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
    • C04B2235/785—Submicron sized grains, 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
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
    • C04B2235/786—Micrometer sized grains, 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
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/79—Non-stoichiometric products, e.g. perovskites (ABO3) with an A/B-ratio other than 1
    • 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
    • C04B2235/80—Phases present in the sintered or melt-cast ceramic products other than the main phase
    • 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
    • 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

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Ceramic Products (AREA)

Abstract

本发明属于陶瓷复合材料的制备技术领域，具体涉及一种氧化铝/钛硅碳复合材料的制备方法。所述的复合材料由钛铝碳（Ti3AlC2），一氧化硅（SiO）均匀接触，真空烧结即可。本发明通过铝和硅的相互扩散，得到氧化铝/钛硅碳复合材料。本发明制备的复合材料具有高致密性，且性能稳定，复合材料中，氧化铝通过钛铝碳和一氧化硅反应生成的，能均匀包覆在钛硅碳晶体的表面，形成一种较为致密的氧化膜，阻碍了基体与外界的物质交换，提高了符合材料整体的抗氧化性能，钛硅碳又增强了复合材料的韧性，制备的复合材料纯度较高，烧结温度较低，并且具备较高的抗弯强度本发明工艺简单，易于工业化生产。

Description

一种氧化铝/钛硅碳复合材料的制备方法
技术领域
本发明属于陶瓷基复合材料领域，具体涉及一种以一氧化硅/钛铝碳(SiO/Ti3AlC2)为原料制备氧化铝/钛硅碳（Al2O3/Ti3SiC2）复合材料的制备方法。
背景技术
氧化铝因其高熔点，高强度，抗氧化，耐高温的优点，是一种极具前景的陶瓷基体材料。但是，氧化铝陶瓷的韧性较低，限制了在工业领域中的应用。MAX陶瓷，MAX相是指三元过渡族金属碳化物或氮化物，其化学通式为“Mn+1AXn”，其中M代表过渡族金属元素，A代表ⅢA或ⅣA族元素，X代表C或N, n=1～3，在陶瓷材料中具备较高韧性，而且MAX相陶瓷的热膨胀系数与氧化铝比较接近，适合与氧化铝陶瓷做结合使用，优势互补，以期获得的具备更好力学性能的新型结构材料。
MAX相陶瓷特别是钛硅碳陶瓷材料与氧化铝的结合已有研究，但是，目前，直接使用钛硅碳与氧化铝粉体制备致密的陶瓷复合材料所需烧结温度较高，约1450℃；钛硅碳与氧化铝界面处无明显反应；容易发生分解，产生碳化钛等杂质。
发明内容
针对现阶段氧化铝/钛硅碳陶瓷复合材料合成中存在的问题，本发明提供了一种氧化铝/钛硅碳复合材料的制备方法，该方法使用钛铝碳/一氧化硅为原材料制备出钛硅碳/氧化铝复合材料，具有较高的抗弯强度。
本发明为了实现上述目的所采用的技术方案为：
一种氧化铝/钛硅碳复合材料的制备方法，所述复合材料以钛铝碳Ti3AlC2粉和一氧化硅SiO粉为原料制备而成。
上述制备方法具体包括以下步骤：
（1）将原料钛铝碳Ti3AlC2粉和一氧化硅SiO粉采用混合均匀，得混合料；
（2）将混合料进行保温加压烧结，保温加压程序结束后随炉降温，降温后关闭真空系统，得到薄饼状氧化铝/钛硅碳复合材料。
进一步的，步骤（1）中，所述钛铝碳的粒径为3-15 μm，一氧化硅的粒径为0.5-5μm，纯度为99.9%。
进一步的，步骤（1）中，所述混合方法为将钛铝碳粉、一氧化硅粉混合，进行球磨混合。
上述混合方法中，钛铝碳与一氧化硅的摩尔比例为1：0.5-1.5。
进一步的，步骤（2）中，所述保温烧结为首先以1-10℃的升温速率升温至1200℃，然后以5-20℃/min的升温速率升温至1250 ℃-1350 ℃，保温1.5-3 h，烧结压力为25-35MPa。
本发明是通过化学反应使一种成本较低的MAX相材料（钛铝碳）转化为另一种MAX相（钛硅碳）材料，同时生成氧化铝的方法。
本发明的有益效果
1、本发明制备的复合材料具有高致密性，且性能稳定，复合材料中，氧化铝通过钛铝碳和一氧化硅反应生成的，能均匀包覆在钛硅碳晶体的表面，形成一种较为致密的氧化膜，阻碍了基体与外界的物质交换，提高了符合材料整体的抗氧化性能，钛硅碳又增强了复合材料的韧性，制备的复合材料纯度较高，烧结温度较低，并且具备较高的抗弯强度
2、本发明工艺简单，易于工业化生产。
附图说明
图1为本发明利用混合法烧结制备的钛硅碳/氧化铝复合材料的X射线衍射图谱。
图2为本发明利用混合法烧结制备的钛硅碳/氧化铝复合材料的微观图像。
图3为本发明利用混合法烧结制备的钛硅碳/氧化铝复合材料的元素分析图。
具体实施方式
下面通过实例对本发明做进一步地阐述，需要强调的是，下述说明仅是为了解释本发明，并不对其内容进行限定。
实施例1
（1）将称得44.22g的粒径10微米左右的钛铝碳（Ti3AlC2）和10.01g的粒径1-5微米的的氧化硅（SiO）加入到行星式球磨机钢罐中，形成钛铝碳与一氧化硅摩尔比1：1左右的混合料，共计约54.23g，用玻璃棒搅拌，使混合料更加均匀；然后放入108.81g的钢球，使得混合料与球的质量比大致为1：2；
（2）将步骤（1）中装有混合料的行星式球磨机钢罐放入行星式球磨机，设置球磨速度70r/min，每30 min暂停10 min，共计球磨时间2 h，暂停时间30 min。球磨完成后，取出混合料；
（3）将步骤（2）中得到得混合料，以下“压头-垫片-碳纸-混合料-碳纸-垫片-上压头”的结构，全部装入直径约45 mm 空心圆柱型石墨模具，放入真空热压炉，打开真空系统抽真空，然后以10 ℃/分钟的升温速率升至1200 ℃，再以5℃ /分钟的升温速率升至1300℃，在1300 ℃时保温120分钟，烧结压力为30 MPa，温度升至1300℃前开启加压程序，保压120分钟。保温加压程序结束后随炉降温，降温至200 ℃时，关闭真空系统，得到薄饼状氧化铝/钛硅碳复合材料。
（4）使用砂纸和抛光机将步骤（3）中的薄饼状氧化铝/钛硅碳复合材料的表面抛光去除与样品表面结合的碳纸，得到可用的样品。
实施例2
（1）将称得43.92g的粒径8微米左右的钛铝碳（Ti3AlC2）和9.99g的粒径1-5微米一氧化硅（SiO）加入到行星式球磨机钢罐中，形成钛铝碳与一氧化硅摩尔比1：1左右的混合料，共计约53.91g，用玻璃棒搅拌，使混合料更加均匀。然后放入107.54g的钢球，使得混合料与球的质量比大致为1：2。
（2）将步骤（1）中装有混合料的行星式球磨机钢罐放入行星式球磨机，设置球磨速度70r/min，每30 min暂停10 min，共计球磨时间2 h，暂停时间30 min。球磨完成后，取出混合料。
（3）将步骤（2）中得到得混合料，以下“压头-垫片-碳纸-混合料-碳纸-垫片-上压头”的结构，全部装入直径约45 mm 空心圆柱型石墨模具，放入真空热压炉，打开真空系统抽真空，然后以8 ℃/分钟的升温速率升至1200 ℃，再以5℃ /分钟的升温速率升至1340℃，在1340 ℃时保温120分钟，烧结压力为30 MPa，温度升至1340℃前开启加压程序，保压120分钟。保温加压程序结束后随炉降温，降温至200 ℃时，关闭真空系统，得到薄饼状氧化铝/钛硅碳复合材料。
（4）使用砂纸和抛光机将步骤（3）中的薄饼状氧化铝/钛硅碳复合材料的表面抛光去除与样品表面结合的碳纸，得到可用的样品。
实施例3
（1）将称得44.13g的粒径10微米左右的钛铝碳（Ti3AlC2）和10.82g的粒径1-5微米一氧化硅（SiO）加入到行星式球磨机钢罐中，形成钛铝碳与一氧化硅摩尔比1：1左右的混合料，共计约54.95g，用玻璃棒搅拌，使混合料更加均匀。然后放入110.69g的钢球，使得混合料与球的质量比大致为1：2。
（2）将步骤（1）中装有混合料的行星式球磨机钢罐放入行星式球磨机，设置球磨速度70r/min，每30 min暂停10 min，共计球磨时间2 h，暂停时间30 min。球磨完成后，取出混合料。
（3）将步骤（2）中得到得混合料，以下“压头-垫片-碳纸-混合料-碳纸-垫片-上压头”的结构，全部装入直径约45 mm 空心圆柱型石墨模具，放入真空热压炉，打开真空系统抽真空，然后以12 ℃/分钟的升温速率升至1200 ℃，再以5℃ /分钟的升温速率升至1280℃，在1280 ℃时保温120分钟，烧结压力为35 MPa，温度升至1280℃前开启加压程序，保压120分钟。保温加压程序结束后随炉降温，降温至200 ℃时，关闭真空系统，得到薄饼状氧化铝/钛硅碳复合材料。
（4）使用砂纸和抛光机将步骤（3）中的薄饼状氧化铝/钛硅碳复合材料的表面抛光去除与样品表面结合的碳纸，得到可用的样品。
实施例4
（1）将称得44.03g的粒径12微米左右的钛铝碳（Ti3AlC2）和10.55g的粒径0.5-3微米一氧化硅（SiO）加入到行星式球磨机钢罐中，形成钛铝碳与一氧化硅摩尔比1：1左右的混合料，共计约54.58g，用玻璃棒搅拌，使混合料更加均匀。然后放入109.9g的钢球，使得混合料与球的质量比大致为1：2。
（2）将步骤（1）中装有混合料的行星式球磨机钢罐放入行星式球磨机，设置球磨速度70r/min，每30 min暂停10 min，共计球磨时间2 h，暂停时间30 min。球磨完成后，取出混合料。
（3）将步骤（2）中得到得混合料，以下“压头-垫片-碳纸-混合料-碳纸-垫片-上压头”的结构，全部装入直径约45 mm 空心圆柱型石墨模具，放入真空热压炉，打开真空系统抽真空，然后以1 ℃/分钟的升温速率升至1200 ℃，再以5℃ /分钟的升温速率升至1280℃，在1280 ℃时保温100分钟，烧结压力为30 MPa，温度升至1280℃前开启加压程序，保压100分钟。保温加压程序结束后随炉降温，降温至200 ℃时，关闭真空系统，得到薄饼状氧化铝/钛硅碳复合材料。
（4）使用砂纸和抛光机将步骤（3）中的薄饼状氧化铝/钛硅碳复合材料的表面抛光去除与样品表面结合的碳纸，得到可用的样品。
效果实施例
（一）将实施例1-4制备的复合材料进行抗弯强度检测，具体检测结果见表1。
抗弯强度检测使用三点弯曲法测试试样的弯曲强度。首先将烧结后的陶瓷圆片放到磨床上粗磨，目的是除去样品表面覆盖的石墨纸和杂质，并将样品表面大致磨平；然后将大致磨平的样品进行抛光，最后将抛光后的试样用线切割机切成所需要的试样条，试样条的表面光滑，无肉眼可见缺陷，尺寸为长36mm，宽4mm，高3mm。试样测试实际跨距为30mm。利用电子万能材料试验机对制得的试样进行弯曲强度测试，测试时试验机上压头下压的速度为0.5 mm/min。记录载荷P，计算出抗弯强度。每个样品制备三个试样条测试三次，最后计算均值。
抗弯强度根据以下材料的弯曲强度公式计算：
Figure 302288DEST_PATH_IMAGE001
Figure 647819DEST_PATH_IMAGE002
表1
Figure 611227DEST_PATH_IMAGE003
（二）本发明制备的钛铝碳/一氧化硅球磨混合烧结制备的钛硅碳/氧化铝复合材料的X射线衍射图谱，如图1所示，微观图像及元素分析如图2和图3所示。
图 1为钛铝碳/一氧化硅球磨混合烧结制备的钛硅碳/氧化铝复合材料的X射线衍射图谱。其中的X射线峰揭示了复合材料中的 Ti3SiC2相（*）、Al2O3 相（◆）和非晶相（△）。非晶相对应于图 1 左侧的突起。Ti3SiC2相、Al2O3 相有明确的XRD峰。
图2为钛铝碳/一氧化硅球磨混合烧结制备的钛硅碳/氧化铝复合材料，在抗弯强度测试产生的断面于扫描电子显微镜下的显示出的微观图像。抗弯强度测试产生断面的SEM显微照片，包含长度约10μm的层状晶体结构，和围绕在四周的其他形状的晶体结构。一氧化硅相可能在断裂测试和超声处理过程中被去除。
图3为与图2对应的元素分布图。Ti-Si-C和Al-O的分布是一致的，并且发现来自分解的 Ti3-C2 层的碳。 因此，在 SEM 显微照片中确定多层 Ti3SiC2 被 Al2O3 紧紧包围（图2）。 破碎的 MAX 晶粒中没有明显 Al 信号，这意味着 SiO 可以将粒径为 10 μm 的Ti3AlC2 转化为层状Ti3SiC2。

Claims (3)

1.一种氧化铝/钛硅碳复合材料的制备方法，其特征在于，所述复合材料以钛铝碳Ti3AlC2粉和一氧化硅SiO粉为原料制备而成；
具体包括以下步骤：
（1）将原料钛铝碳Ti3AlC2粉和一氧化硅SiO粉混合均匀，得混合料；
所述钛铝碳与一氧化硅的摩尔比例为1：0.5-1.5；
（2）将混合料进行保温加压烧结，保温加压程序结束后随炉降温，降温后关闭真空系统，得到薄饼状氧化铝/钛硅碳复合材料；
所述保温烧结为首先以1-10℃的升温速率升温至1200℃，然后以5-20℃/min的升温速率升温至1250 ℃-1350 ℃，保温1.5-3 h，烧结压力为25-35MPa。
2.根据权利要求1所述的制备方法，其特征在于，步骤（1）中，所述钛铝碳的粒径为3-15μm，一氧化硅的粒径为0.5-5μm，纯度为99.9%。
3.根据权利要求1所述的制备方法，其特征在于，步骤（1）中，所述混合料采用球磨法进行混合。
CN202110987687.2A 2021-08-26 2021-08-26 一种氧化铝/钛硅碳复合材料的制备方法 Active CN113735585B (zh)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN202110987687.2A CN113735585B (zh) 2021-08-26 2021-08-26 一种氧化铝/钛硅碳复合材料的制备方法
US17/892,081 US11673841B2 (en) 2021-08-26 2022-08-21 Preparation method for alumina/titanium silicon carbide composite matertal

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110987687.2A CN113735585B (zh) 2021-08-26 2021-08-26 一种氧化铝/钛硅碳复合材料的制备方法

Publications (2)

Publication Number Publication Date
CN113735585A CN113735585A (zh) 2021-12-03
CN113735585B true CN113735585B (zh) 2022-06-10

Family

ID=78732993

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110987687.2A Active CN113735585B (zh) 2021-08-26 2021-08-26 一种氧化铝/钛硅碳复合材料的制备方法

Country Status (2)

Country Link
US (1) US11673841B2 (zh)
CN (1) CN113735585B (zh)

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6461989B1 (en) * 1999-12-22 2002-10-08 Drexel University Process for forming 312 phase materials and process for sintering the same
CN1259279C (zh) * 2004-06-23 2006-06-14 北京交通大学 一种以铝为添加剂的钛硅碳块体材料及其制备方法
CN100381396C (zh) * 2005-11-23 2008-04-16 中国科学院金属研究所 一种铝碳化钛-碳化钛/氧化铝复合材料及其制备方法
US20110097582A1 (en) * 2008-01-21 2011-04-28 Sumitomo Chemical Company, Limited Aluminum magnesium titanate-alumina composite ceramics
CN104099488B (zh) * 2014-07-24 2016-07-06 北京交通大学 一种无压烧结-加压致密化制备钛铝碳颗粒增强锌铝基复合材料的方法
CN108232144B (zh) * 2017-12-25 2020-09-25 北方奥钛纳米技术有限公司 一种改性硅碳复合电极材料及其制备方法
CN110105071A (zh) * 2019-06-06 2019-08-09 南通通州湾新材料科技有限公司 一种硅化木外观结构件的制备方法及其手机背板
CN113839016B (zh) * 2021-08-23 2023-08-01 惠州锂威新能源科技有限公司 一种负极材料及其制备方法
CN113823781A (zh) * 2021-08-23 2021-12-21 惠州锂威新能源科技有限公司 一种复合负极材料及其制备方法

Also Published As

Publication number Publication date
US11673841B2 (en) 2023-06-13
CN113735585A (zh) 2021-12-03
US20230075594A1 (en) 2023-03-09

Similar Documents

Publication Publication Date Title
Heydari et al. Comparing the effects of different sintering methods for ceramics on the physical and mechanical properties of B4C–TiB2 nanocomposites
CN110128146B (zh) 一种具有多功能的碳化硼基复相陶瓷及其反应热压烧结制备方法
JPH0776128B2 (ja) 炭化ほう素―アルミニウム及び炭化ほう素―反応性金属サーメット
Li et al. Preparation and mechanical properties of SiC-AlN ceramic alloy
JP2001080964A (ja) 多結晶ＳｉＣ成形体、その製法及びそれからなる応用品
Xiao-Zheng et al. TEM investigation of high-pressure reaction-sintered cBN-Al composites
Ruh et al. Phase and property studies of boron carbide–boron nitride composites
JPS6128627B2 (zh)
JP6908248B2 (ja) 被覆ＳｉＣナノ粒子を用いたＳｉＣセラミックス及びその製造方法
CN109180161B (zh) 一种高纯钛硅化碳/氧化铝复合材料及其制备方法
US5227346A (en) Sialon composites and method of preparing the same
JPH06508339A (ja) 高靱性−高強度焼結窒化ケイ素
CN112110740A (zh) 一种原位反应制备氧化铝基复合生物陶瓷材料的方法及其制得的产品
US5767025A (en) Composite powder comprising silicon nitride and silicon carbide
CN113735585B (zh) 一种氧化铝/钛硅碳复合材料的制备方法
CN115073186B (zh) 一种氮化硅陶瓷烧结体及其制备方法
Solodkyi et al. Low-temperature synthesis of boron carbide ceramics
CN106083002B (zh) 低温烧结原位合成六铝酸镧增强的氧化铝陶瓷及其制备
Kanai et al. Hot-Pressed BN-AlN Ceramic Composites with High Thermal Conductivity. Part III
CN103073317B (zh) 一种铝氮化钛／二硼化钛复合材料及其制备方法
CN113264775A (zh) 致密质复合材料、其制法、接合体及半导体制造装置用构件
Watanabe et al. Fabrication of SiC AlN/Mo functionally gradient material for high temperature use
JP3618211B2 (ja) 六方晶窒化硼素焼結体の製造方法
JP3148559B2 (ja) セラミックス繊維強化タービン翼及びその製造方法
CN102718488A (zh) 一种铪铝硅碳-碳化硅复合材料及其制备方法

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