CN112062572A - 一种高致密度的碳化硅陶瓷及其制备方法和应用 - Google Patents
一种高致密度的碳化硅陶瓷及其制备方法和应用 Download PDFInfo
- Publication number
- CN112062572A CN112062572A CN202010837642.2A CN202010837642A CN112062572A CN 112062572 A CN112062572 A CN 112062572A CN 202010837642 A CN202010837642 A CN 202010837642A CN 112062572 A CN112062572 A CN 112062572A
- Authority
- CN
- China
- Prior art keywords
- silicon carbide
- carbide ceramic
- density
- sintering
- ball milling
- 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
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 46
- 239000000919 ceramic Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000005245 sintering Methods 0.000 claims abstract description 31
- 238000000498 ball milling Methods 0.000 claims abstract description 17
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 16
- 229920003257 polycarbosilane Polymers 0.000 claims abstract description 15
- 238000005336 cracking Methods 0.000 claims abstract description 12
- 239000012298 atmosphere Substances 0.000 claims abstract description 9
- 238000005452 bending Methods 0.000 claims abstract description 9
- 230000001681 protective effect Effects 0.000 claims abstract description 9
- 239000002243 precursor Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000011812 mixed powder Substances 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 3
- 238000005272 metallurgy Methods 0.000 claims description 3
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 2
- 229910052691 Erbium Inorganic materials 0.000 claims description 2
- 229910052693 Europium Inorganic materials 0.000 claims description 2
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 2
- 229910052689 Holmium Inorganic materials 0.000 claims description 2
- 229910052765 Lutetium Inorganic materials 0.000 claims description 2
- 229910052779 Neodymium Inorganic materials 0.000 claims description 2
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 2
- 229910052772 Samarium Inorganic materials 0.000 claims description 2
- 229910052771 Terbium Inorganic materials 0.000 claims description 2
- 229910052775 Thulium Inorganic materials 0.000 claims description 2
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 229910052706 scandium Inorganic materials 0.000 claims description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
- 229910052575 non-oxide ceramic Inorganic materials 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 3
- 238000002679 ablation Methods 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910003443 lutetium oxide Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000001272 pressureless sintering Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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
- C04B35/571—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 from Si-containing polymer precursors or organosilicon monomers
-
- 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
- C04B35/573—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 reaction sintering or recrystallisation
-
- 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
-
- 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
- C04B2235/32—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
-
- 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
- C04B2235/30—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
- C04B2235/3227—Lanthanum 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
- C04B2235/30—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
- C04B2235/3229—Cerium oxides 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
- C04B2235/65—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
- C04B2235/70—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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Ceramic Products (AREA)
Abstract
本发明属于非氧化物陶瓷材料领域，公开了一种高致密碳化硅陶瓷及其制备方法和应用。所述碳化硅陶瓷是以聚碳硅烷作为前驱体，以Al2O3‑Re2O3为烧结助剂，将聚碳硅烷和Al2O3‑Re2O3球磨混合后，保护气氛下，在500～1200℃裂解，所得碳化硅粉体经预压后在1500～1700℃进行烧结制得。本发明制得的SiC陶瓷的致密度为97％以上，维氏硬度为20～30GPa，抗弯强度为700～1200MPa，断裂韧性为6～12MPa·m1/2，在1200℃下高温强度为600～1000MPa。本发明可实现各种结构复杂的大型结构件的制备，大大地降低了制备成本。
Description
技术领域
本发明属于非氧化物陶瓷材料技术领域，更具体地，涉及一种高致密度的碳化硅陶瓷及其制备方法和应用。
背景技术
碳化硅(SiC)陶瓷具有高熔点、高强度、高硬度以及耐腐蚀等优异的性能；尤其是其抗高温烧蚀性能，使其在航空航天飞行器、冶炼窑炉构件等高温应用场景大放异彩。但由于SiC的强共价键，导致其烧结性能差，很难通过自扩散实现烧结致密化，导致烧结的成品致密度较低。
目前，对于SiC陶瓷的制备主要集中在高温、高压条件下制备；然而，以上方法不仅制备成本高，而且不利于大型结构件的成型制备，极大地限制了其应用。为了解决以上问题，通常需要加入各种烧结助剂促进SiC陶瓷的烧结。以上方法虽然可以一定程度上降低SiC陶瓷制备的温度和压力，但是仍然没有从本质上解决SiC陶瓷的低烧结活性。基于以上背景，急需开发一种方法通过改善SiC陶瓷的烧结活性，在温和条件下制备得到致密高性能SiC陶瓷。
发明内容
为了解决上述现有技术存在的不足和缺点，提供一种高致密度的碳化硅陶瓷。
本发明的另一目的在于提供上述高致密度的碳化硅陶瓷的制备方法。该方法是以聚碳硅烷作为前驱体，通过裂解得到高活性的碳化硅，并通过较低温度的烧结制得高致密度的碳化硅陶瓷。
本发明的再一目的在于提供上述高致密度的碳化硅陶瓷的应用。
本发明的目的通过下述技术方案来实现：
一种高致密度的碳化硅陶瓷，所述碳化硅陶瓷是以聚碳硅烷作为前驱体，以Al2O3-Re2O3为烧结助剂，将聚碳硅烷和Al2O3-Re2O3球磨混合后，保护气氛下，在500～1200℃裂解，所得碳化硅粉体经预压后在1500～1700℃进行烧结制得。
优选地，所述的述碳化硅陶瓷的致密度为97％以上，维氏硬度为20～30GPa，抗弯强度为700～1200MPa，断裂韧性为6～12MPa·m1/2，在1200℃下高温强度为600～1000MPa。
优选地，所述Al2O3-Re2O3的纯度为99～99.9wt.％，所述Al2O3-Re2O3的粒径为0.01～2μm。
优选地，所述Re2O3中Re为Sc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb或Lu。
优选地，所述球磨为辊式球磨，是以乙醇为溶剂，以氮化硅球为球磨介质，球磨转速为500～150r/min，所述球磨的时间为8～24h。
优选地，所述聚碳硅烷和烧结助剂的质量比为(17～19)：(1～3)；所述烧结助剂中的Al2O3与Re2O3的质量比为(1～99)：(1～99)。
优选地，所述裂解的升温速率为5～20℃/min，所述烧结的升温速率为5～15℃/min，所述烧结的时间为1～20min。
优选地，所述保护气氛为氮气或氩气。
所述的高致密度的碳化硅陶瓷的制备方法，包括以下具体步骤：
S1.将聚碳硅烷前驱体和烧结助剂Al2O3-Re2O3球磨混合后，保护气氛下，在500～1200℃裂解，得到混合粉体；
S2.将裂解所得混合粉体预压后在保护气氛下1500～1700℃进行无压烧结，制得高致密度的碳化硅陶瓷。
所述的高致密度的碳化硅陶瓷在高温冶金或发动机耐高温零部件领域中的应用。
与现有技术相比，本发明具有以下有益效果：
1.本发明以聚碳硅烷作为前驱体，通过对裂解温度的控制实现SiC烧结活性的调控，从本质上解决SiC烧结活性低的问题。
2.本发明可实现低温、低压条件下致密SiC陶瓷的制备，极大地降低其制备成本。
3.本发明可实现各种形状复杂大型结构件的制备，极大地促进SiC陶瓷的工程应用。
具体实施方式
下面结合具体实施例进一步说明本发明的内容，但不应理解为对本发明的限制。若未特别指明，实施例中所用的技术手段为本领域技术人员所熟知的常规手段。除非特别说明，本发明采用的试剂、方法和设备为本技术领域常规试剂、方法和设备。
实施例1
1.制备：
(1)以产率为60wt％的聚碳硅烷作为前驱体，以Al2O3-Y2O3为烧结助剂，将质量百分比为90％、5％和5％的聚碳硅烷、Al2O3与Y2O3用Si3N4球在辊式球磨下，以100r/min的转数进行球磨混合8h，制得混合粉体；
(2)在氮气气氛下，将混合粉体以5℃/min升温至800℃保温1h，得到裂解粉体；
(3)将裂解粉体装入烧结模具，经10MPa预压后放入烧结设备中，在氮气气氛下进行无压烧结，以10℃/min升温至1600℃，保温10min，制得致密的碳化硅(SiC)陶瓷。
2.性能测试：本实施例所得的碳化硅陶瓷的致密度为98％，维氏硬度为25GPa，抗弯强度为1000MPa，断裂韧性为8MPa·m1/2，在1200℃下高温强度为800MPa。
实施例2
与实施例1不同的在于：步骤(3)中所述碳化硅是以15℃/min升温至1700℃。
本实施例的碳化硅陶瓷的致密度为97％，维氏硬度为24GPa，抗弯强度为900MPa，断裂韧性为7MPa·m1/2，在1200℃下高温强度为700MPa。
实施例3
与实施例1不同的在于：步骤(1)中所述烧结助剂为Al2O3-Lu2O3，所述聚碳硅烷、Al2O3与Re2O3的质量百分比为94％、3％与3％。
本实施例所得的碳化硅陶瓷的致密度为99％，维氏硬度为26GPa，抗弯强度为1000MPa，断裂韧性为9MPa·m1/2，在1200℃下高温强度为800MPa。
实施例4
与实施例1不同的在于：步骤(3)中所述预压的压力为30MPa。
本实施例所得的碳化硅陶瓷的致密度为99％，维氏硬度为28GPa，抗弯强度为1000MPa，断裂韧性为7MPa·m1/2，在1200℃下高温强度为800MPa。
实施例5
与实施例1不同的在于：
步骤(3)中所述升温速率为200℃/min，所述保温时间为20min。
本实施例所得的碳化硅陶瓷的致密度为98％，维氏硬度为24GPa，抗弯强度为1000MPa，断裂韧性为10MPa·m1/2，在1200℃下高温强度为700MPa。
本发明的碳化硅陶瓷的致密度为97％以上，维氏硬度为20～30GPa，抗弯强度为700～1200MPa，断裂韧性为6～12MPa·m1/2，在1200℃下高温强度为600～1000MPa，可应用在高温冶金或发动机耐高温零部件领域中。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合和简化，均应为等效的置换方式，都包含在本发明的保护范围之内。
Claims (10)
1.一种高致密度的碳化硅陶瓷，其特征在于，所述碳化硅陶瓷是以聚碳硅烷作为前驱体，以Al2O3-Re2O3为烧结助剂，将聚碳硅烷和Al2O3-Re2O3球磨混合后，保护气氛下，在500～1200℃裂解，所得碳化硅粉体经预压后在1500～1700℃进行烧结制得。
2.根据权利要求1所述的高致密度的碳化硅陶瓷，其特征在于，所述的碳化硅陶瓷的致密度为97％以上，维氏硬度为20～30GPa，抗弯强度为700～1200MPa，断裂韧性为6～12MPa·m1/2，在1200℃下高温强度为600～1000MPa。
3.根据权利要求1所述的高致密度的碳化硅陶瓷，其特征在于，所述Al2O3-Re2O3的纯度为99～99.9wt.％，所述Al2O3-Re2O3的粒径为0.01～2μm。
4.根据权利要求3所述的高致密度的碳化硅陶瓷，其特征在于，所述Re2O3中Re为Sc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb或Lu。
5.根据权利要求1所述的高致密度的碳化硅陶瓷，其特征在于，所述球磨为辊式球磨，是以乙醇为溶剂，以氮化硅球为球磨介质，球磨转速为500～150r/min，所述球磨的时间为8～24h。
6.根据权利要求1所述的高致密度的碳化硅陶瓷，其特征在于，所述聚碳硅烷和烧结助剂的质量比为(17～19)：(1～3)；所述烧结助剂中的Al2O3与Re2O3的质量比为(1～99)：(1～99)。
7.根据权利要求1所述的高致密度的碳化硅陶瓷，其特征在于，所述裂解的升温速率为5～20℃/min，所述烧结的升温速率为5～15℃/min，所述烧结的时间为1～20min。
8.根据权利要求1所述的高致密度的碳化硅陶瓷，其特征在于，所述保护气氛为氮气或氩气。
9.根据权利要求1～8任一项所述的高致密度的碳化硅陶瓷的制备方法，其特征在于，包括以下具体步骤：
S1.将聚碳硅烷前驱体和烧结助剂Al2O3-Re2O3球磨混合后，保护气氛下，在500～1200℃裂解，得到混合粉体；
S2.将裂解所得混合粉体预压后在保护气氛下1500～1700℃进行无压烧结，制得高致密度的碳化硅陶瓷。
10.权利要求1～8任一项所述的高致密度的碳化硅陶瓷在高温冶金或发动机耐高温零部件领域中的应用。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010837642.2A CN112062572A (zh) | 2020-08-19 | 2020-08-19 | 一种高致密度的碳化硅陶瓷及其制备方法和应用 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010837642.2A CN112062572A (zh) | 2020-08-19 | 2020-08-19 | 一种高致密度的碳化硅陶瓷及其制备方法和应用 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112062572A true CN112062572A (zh) | 2020-12-11 |
Family
ID=73661425
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010837642.2A Pending CN112062572A (zh) | 2020-08-19 | 2020-08-19 | 一种高致密度的碳化硅陶瓷及其制备方法和应用 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112062572A (zh) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115650751A (zh) * | 2022-10-13 | 2023-01-31 | 广东核电合营有限公司 | 纤维强韧化的碳化硅包壳及其制备方法 |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4105455A (en) * | 1976-08-17 | 1978-08-08 | Kyoto Ceramic Kabushiki Kaisha | Method of producing dense sintered silicon carbide body from polycarbosilanes |
| US4374793A (en) * | 1977-01-27 | 1983-02-22 | Kyoto Ceramic Kabushiki Kaisha | Method of producing dense sintered silicon carbide body from polycarbosilane |
| US4962069A (en) * | 1988-11-07 | 1990-10-09 | Dow Corning Corporation | Highly densified bodies from preceramic polysilazanes filled with silicon carbide powders |
| JPH05132361A (ja) * | 1991-11-08 | 1993-05-28 | Toyota Motor Corp | 窒化ケイ素焼結体の製造方法 |
| CN101928148A (zh) * | 2009-07-20 | 2010-12-29 | 宁波大学 | 一种基于硅烷偶联剂低温高致密碳化硅陶瓷制造方法 |
| CN104140265A (zh) * | 2014-07-28 | 2014-11-12 | 中国科学院上海硅酸盐研究所 | 采用液相烧结制备以氧化锆为增韧相的碳化硅陶瓷的方法 |
| CN108455988A (zh) * | 2018-05-11 | 2018-08-28 | 广东工业大学 | 一种碳化硅陶瓷及其制备方法 |
| CN110436930A (zh) * | 2019-08-05 | 2019-11-12 | 广东工业大学 | 一种高性能纳米SiC陶瓷及其制备方法和应用 |
| CN110877980A (zh) * | 2019-11-13 | 2020-03-13 | 中国科学院上海硅酸盐研究所 | 一种高强度碳化硅/氮化硅复相陶瓷及其制备方法 |
-
2020
- 2020-08-19 CN CN202010837642.2A patent/CN112062572A/zh active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4105455A (en) * | 1976-08-17 | 1978-08-08 | Kyoto Ceramic Kabushiki Kaisha | Method of producing dense sintered silicon carbide body from polycarbosilanes |
| US4374793A (en) * | 1977-01-27 | 1983-02-22 | Kyoto Ceramic Kabushiki Kaisha | Method of producing dense sintered silicon carbide body from polycarbosilane |
| US4962069A (en) * | 1988-11-07 | 1990-10-09 | Dow Corning Corporation | Highly densified bodies from preceramic polysilazanes filled with silicon carbide powders |
| JPH05132361A (ja) * | 1991-11-08 | 1993-05-28 | Toyota Motor Corp | 窒化ケイ素焼結体の製造方法 |
| CN101928148A (zh) * | 2009-07-20 | 2010-12-29 | 宁波大学 | 一种基于硅烷偶联剂低温高致密碳化硅陶瓷制造方法 |
| CN104140265A (zh) * | 2014-07-28 | 2014-11-12 | 中国科学院上海硅酸盐研究所 | 采用液相烧结制备以氧化锆为增韧相的碳化硅陶瓷的方法 |
| CN108455988A (zh) * | 2018-05-11 | 2018-08-28 | 广东工业大学 | 一种碳化硅陶瓷及其制备方法 |
| CN110436930A (zh) * | 2019-08-05 | 2019-11-12 | 广东工业大学 | 一种高性能纳米SiC陶瓷及其制备方法和应用 |
| CN110877980A (zh) * | 2019-11-13 | 2020-03-13 | 中国科学院上海硅酸盐研究所 | 一种高强度碳化硅/氮化硅复相陶瓷及其制备方法 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115650751A (zh) * | 2022-10-13 | 2023-01-31 | 广东核电合营有限公司 | 纤维强韧化的碳化硅包壳及其制备方法 |
| CN115650751B (zh) * | 2022-10-13 | 2023-10-31 | 广东核电合营有限公司 | 纤维强韧化的碳化硅包壳及其制备方法 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112608164B (zh) | 连接钎料及其制备方法、碳化硅包壳连接方法 | |
| CN106904977B (zh) | 一种两步烧结法制备表硬心韧Si3N4陶瓷材料的方法 | |
| CN110818428B (zh) | 一种共晶增强增韧氮化硅陶瓷的制备方法 | |
| CN110483060B (zh) | 一种高热导率氮化硅陶瓷及其制备方法 | |
| CN114315359B (zh) | 一种利用固溶耦合法制备高强韧复相高熵陶瓷的方法和应用 | |
| CN108439995B (zh) | 一种复相陶瓷及其制备方法 | |
| CN114163244A (zh) | 一种外硬内韧氮化硅陶瓷及其制备方法 | |
| CN111302809B (zh) | 一种高热导率、高强度氮化硅陶瓷材料及其制备方法 | |
| CN112062572A (zh) | 一种高致密度的碳化硅陶瓷及其制备方法和应用 | |
| CN116239387A (zh) | 利用中/高熵多元稀土烧结助剂的高强度氮化硅制备方法 | |
| CN111393170A (zh) | 一种通过多因素优化制备高致密度氮化硅陶瓷的方法及制备的氮化硅陶瓷 | |
| CN112062574B (zh) | 一种高性能纳米碳化硅陶瓷及其制备方法和应用 | |
| CN114671689A (zh) | 一种热压液相烧结碳化硼复合陶瓷及其制备方法 | |
| CN101551012A (zh) | 含碳的碳化硅密封环及其制备方法 | |
| CN113880557A (zh) | AL2O3-cBN基陶瓷刀具材料及其制备方法 | |
| CN108585907B (zh) | 一种Cr2AlC改性的自愈合碳化硅陶瓷基复合材料的制备方法 | |
| CN109467442B (zh) | 一种氮化硅陶瓷及其制备方法 | |
| CN113929463B (zh) | 一种烧结法制备钛副族碳氮化物固溶体复相陶瓷材料的方法 | |
| JPS605079A (ja) | サイアロン基セラミツクスの製造法 | |
| CN1552667A (zh) | 碳化物陶瓷防弹板材料及其陶瓷防弹板的制造方法 | |
| HIROSAKI et al. | Dense silicon nitride containing low amounts of Y2O3 and Nd2O3 | |
| CN114394837A (zh) | 一种抗氧化性的二硼化物-碳化物固溶体陶瓷的制备方法和应用 | |
| CN100430339C (zh) | 陶瓷滑动轴承及其制造方法 | |
| CN111099897A (zh) | 一种碳化硅复合材料及其制备方法 | |
| CN1552668A (zh) | 陶瓷滑动轴承及其制造方法 |
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 | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20201211 |