CN113307644A - 一种氮化改性反应烧结碳化硅陶瓷表面的方法 - Google Patents
一种氮化改性反应烧结碳化硅陶瓷表面的方法 Download PDFInfo
- Publication number
- CN113307644A CN113307644A CN202110669667.0A CN202110669667A CN113307644A CN 113307644 A CN113307644 A CN 113307644A CN 202110669667 A CN202110669667 A CN 202110669667A CN 113307644 A CN113307644 A CN 113307644A
- Authority
- CN
- China
- Prior art keywords
- silicon carbide
- reaction
- ceramic
- sintering
- mixing
- 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 131
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 131
- 239000000919 ceramic Substances 0.000 title claims abstract description 56
- 238000005245 sintering Methods 0.000 title claims abstract description 53
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 47
- 238000005121 nitriding Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title description 4
- 238000002156 mixing Methods 0.000 claims abstract description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000011230 binding agent Substances 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 20
- 239000002270 dispersing agent Substances 0.000 claims abstract description 18
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 16
- 239000006229 carbon black Substances 0.000 claims abstract description 16
- 239000004917 carbon fiber Substances 0.000 claims abstract description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims abstract description 8
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 8
- 239000001768 carboxy methyl cellulose Substances 0.000 claims abstract description 8
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims abstract description 8
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims abstract description 8
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 8
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 8
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 8
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 8
- 238000004381 surface treatment Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims description 18
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 8
- 235000015895 biscuits Nutrition 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 238000000855 fermentation Methods 0.000 claims description 5
- 230000004151 fermentation Effects 0.000 claims description 5
- 238000012986 modification Methods 0.000 claims description 5
- 230000004048 modification Effects 0.000 claims description 5
- 239000002985 plastic film Substances 0.000 claims description 5
- 229920006255 plastic film Polymers 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 229910052710 silicon Inorganic materials 0.000 abstract description 15
- 239000010703 silicon Substances 0.000 abstract description 15
- 238000002360 preparation method Methods 0.000 abstract description 11
- 230000007797 corrosion Effects 0.000 abstract description 10
- 238000005260 corrosion Methods 0.000 abstract description 10
- 229910017464 nitrogen compound Inorganic materials 0.000 abstract 1
- 150000002830 nitrogen compounds Chemical class 0.000 abstract 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 13
- 239000000853 adhesive Substances 0.000 description 6
- 230000001070 adhesive effect Effects 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000006011 modification reaction Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000001272 pressureless sintering Methods 0.000 description 1
- 239000002296 pyrolytic carbon Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 238000002490 spark plasma sintering Methods 0.000 description 1
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
- C04B35/573—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
-
- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5053—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
- C04B41/5062—Borides, Nitrides or Silicides
- C04B41/5066—Silicon 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
-
- 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
- C04B2235/424—Carbon black
-
- 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
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5216—Inorganic
- C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
- C04B2235/5248—Carbon, e.g. graphite
-
- 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
- C04B2235/602—Making the green bodies or pre-forms by moulding
- C04B2235/6021—Extrusion moulding
-
- 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
- C04B2235/656—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
- C04B2235/658—Atmosphere during thermal treatment
- C04B2235/6581—Total pressure below 1 atmosphere, e.g. vacuum
-
- 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)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Ceramic Products (AREA)
Abstract
本发明涉及一种表面氮化改性的反应烧结碳化硅陶瓷及其制备方法，反应烧结碳化硅陶瓷包括碳化硅、炭黑、碳纤维、粘结剂、分散剂、去离子水；所述粘结剂为羧甲基纤维素和PAF‑Ⅱ型粉状粘结剂以任意比混合；所述分散剂为聚乙二醇和聚乙烯吡咯烷酮以任意比混合。制备方法包括混料、醒料、烧结和表面处理。本发明是在一定压力下通入流动的氮气，使氮气与游离硅反应生成硅和氮的化合物，提高反应烧结碳化硅的使用寿命和耐腐蚀能力。
Description
技术领域
本发明涉及一种氮化改性反应烧结碳化硅陶瓷表面的方法，属于碳化硅改性技术领域。
背景技术
碳化硅具有高硬度、高温强度大、抗氧化性好、热稳定性好、热膨胀系数低、热导率大及耐腐蚀性好等优良特性，因此，可以用作密封环、研磨介质、研磨盘、防弹板、喷嘴、磁力泵泵件、窑炉中的辊棒等。对于碳化硅陶瓷的制备有无压烧结、热压烧结、热等静压烧结、放电等离子烧结、反应烧结等，其中反应烧结制备碳化硅陶瓷，其烧结温度低、制品的尺寸收缩小、致密度高、经济效益好、工业成本较低，但是由于反应烧结需利用熔融硅浸渗含碳的碳化硅陶瓷素坯，使所制得的陶瓷制品中含有游离硅。由于硅的熔点为1400℃，因此游离硅在反应烧结碳化硅中的存在缩短了反应烧结碳化硅在高温下的使用寿命而且其耐腐蚀性能也大幅度下降。
专利文献CN110304933A公开了PyC-SiCW表面的热解碳涂层在反应烧结过程中与液硅发生反应在PyC-SiCW表面原位生成一层SiC涂层，SiC涂层将SiCW与高温液硅相互隔离，避免了高温下液硅对SiCW的侵蚀损伤。本发明采用的是在陶瓷的表面形成SiC涂层来增加其陶瓷的抗侵蚀性；而本发明的目的是减少游离硅的含量，提高反应烧结碳化硅的耐腐蚀性，就是将反应烧结碳化硅陶瓷中的游离硅和氮气反应生成氮化硅。目前对于反应烧结碳化硅表面处理的文献很少，尤其是采用氮气来处理反应烧结碳化硅陶瓷的表面。
发明内容
本发明针对反应烧结碳化硅作为窑炉辊棒，在高温下抗锂电腐蚀性差的问题，提出一种低成本、易实现的一种表面氮化改性的反应烧结碳化硅陶瓷及其制备方法。本发明的技术方案如下：
一种表面氮化改性的反应烧结碳化硅陶瓷，包括以下按重量份数计的原料：
碳化硅5-40份、炭黑2-7份、碳纤维3-8份、粘结剂2-6份、分散剂0.1-0.4份、去离子水10-40份；
所述粘结剂为羧甲基纤维素和PAF-Ⅱ型粉状粘结剂以任意比混合；所述分散剂为聚乙二醇和聚乙烯吡咯烷酮以任意比混合。
优选的，所述碳化硅选自F90的碳化硅、F120的碳化硅、F180的碳化硅和F1200的碳化硅的混合物。
优选的，所述F90的碳化硅、F120的碳化硅、F180的碳化硅和F1200的碳化硅的重量比为1:2:1:2；所述羧甲基纤维素和PAF-Ⅱ型粉状粘结剂以1:1的重量比混合；所述聚乙二醇和聚乙烯吡咯烷酮以2:1的重量比混合；所述炭黑和碳纤维的粒径分别为0.5-1μm和7-8μm。
上述表面氮化改性的反应烧结碳化硅陶瓷的制备方法，步骤如下：
（1）混料
取去离子水，将分散剂和粘结剂充分溶解，再称取F90的碳化硅、F120的碳化硅、F180的碳化硅、F1200的碳化硅、炭黑、碳纤维，在常温下利用滚筒混料机混料8-20h，将各组分混合均匀，获得混合物A；
（2）醒料
将步骤（1）所制得的混合物A放置到塑料膜内常温醒料10-24h，将醒好的混合物A放入挤出机中挤出所需陶瓷坯体；
（3）烧结
将步骤（2）制得的陶瓷素坯放置于真空反应烧结炉中，在1500-1850℃下烧结5-12h，制得碳化硅陶瓷；
（4）表面处理
将反应烧结碳化硅放置到高温炉中，在加热同时通入流动的高纯氮气，进而生成表面氮化改性的反应烧结碳化硅陶瓷；氮气在高温下与反应烧结碳化硅表面的游离硅反应生成氮和硅的化合物，以增加反应烧结碳化硅耐锂电腐蚀的性能。
进一步的，所述步骤（4）中将反应烧结碳化硅放置到高温炉中，以流量为15-25m3/h向高温炉中通入流动性的高纯氮气，加热温度为1250-1350℃，保温时间为4-8h。
本发明与现有技术相比具有以下优点：
本发明通过复合粘结剂、复合分散剂、复合碳源、不同粒径的碳化硅及去离子水为原料，进行混料、醒料、烧结、表面处理，制得反应烧结的碳化硅陶瓷。将制得的反应烧结陶瓷放入高温炉中在一定压力下通入流动的氮气，在一定的热处理温度和时间下，使氮气和游离硅反应生成氮和硅的化合物，提高反应烧结碳化硅的使用寿命和耐腐蚀能力。
附图说明
图1为1350℃氮化处理的反应烧结碳化硅的XPS图；
图2 为电池材料腐蚀图片，其中，2A为未处理碳化硅烧结锂电池材料的腐蚀图片；2B为为本发明氮化处理的碳化硅烧结锂电池材料的腐蚀图片。
具体实施方式
下面结合具体实施例来进一步描述本发明，本发明的优点和特点将会随着描述而更为清楚。但实施例仅是范例性的，并不对本发明的范围构成任何限制。本领域技术人员应该理解的是，在不偏离本发明的精神和范围下可以对本发明技术方案的细节和形式进行修改或替换，但这些修改和替换均落入本发明的保护范围内。
实施例1：一种表面氮化改性的反应烧结碳化硅陶瓷及其制备方法
表面氮化改性的反应烧结碳化硅陶瓷包括以下按重量份数计的原料：
碳化硅30份、炭黑5份、碳纤维5份、粘结剂4份、分散剂0.3份、去离子水20份；
所述碳化硅选自F90的碳化硅、F120的碳化硅、F180的碳化硅和F1200的碳化硅的混合物，其重量比为1:2:1:2；所述粘结剂为羧甲基纤维素和PAF-Ⅱ型粉状粘结剂以1:1的重量比混合；所述分散剂为聚乙二醇和聚乙烯吡咯烷酮以2:1的重量比混合；所述炭黑和碳纤维的粒径分别为0.7μm和7μm。
上述表面氮化改性的反应烧结碳化硅陶瓷的制备方法，步骤如下：
（1）混料
取去离子水，将分散剂和粘结剂充分溶解，再称取F90的碳化硅、F120的碳化硅、F180的碳化硅、F1200的碳化硅、炭黑、碳纤维，在常温下利用滚筒混料机混料10h，将各组分混合均匀，获得混合物A；
（2）醒料
将步骤（1）所制得的混合物A放置到塑料膜内常温醒料18h，将醒好的混合物A放入挤出机中挤出所需陶瓷坯体；
（3）烧结
将步骤（2）制得的陶瓷素坯放置于真空反应烧结炉中，在1600℃下烧结10h，制得碳化硅陶瓷；
（4）表面处理
将反应烧结碳化硅放置到高温炉中，以流量为15m3/h向高温炉中通入流动性的高纯氮气，加热温度为1250℃，保温时间为8h，获得表面氮化改性的反应烧结碳化硅陶瓷。
经检测，该实施例获得表面氮化改性的反应烧结碳化硅陶瓷的弯曲强度为317MPa，断裂韧性为3MPa·m1/2。
实施例2：一种表面氮化改性的反应烧结碳化硅陶瓷及其制备方法
表面氮化改性的反应烧结碳化硅陶瓷包括以下按重量份数计的原料：
碳化硅15份、炭黑4份、碳纤维6份、粘结剂4份、分散剂0.2份、去离子水15份；
所述碳化硅选自F90的碳化硅、F120的碳化硅、F180的碳化硅和F1200的碳化硅的混合物，其重量比为1:2:1:2；所述粘结剂为羧甲基纤维素和PAF-Ⅱ型粉状粘结剂以2:1的重量比混合；所述分散剂为聚乙二醇和聚乙烯吡咯烷酮以2:1的重量比混合；所述炭黑和碳纤维的粒径分别为0.6μm和8μm。
上述表面氮化改性的反应烧结碳化硅陶瓷的制备方法，步骤如下：
（1）混料
取去离子水，将分散剂和粘结剂充分溶解，再称取F90的碳化硅、F120的碳化硅、F180的碳化硅、F1200的碳化硅、炭黑、碳纤维，在常温下利用滚筒混料机混料15h，将各组分混合均匀，获得混合物A；
（2）醒料
将步骤（1）所制得的混合物A放置到塑料膜内常温醒料15h，将醒好的混合物A放入挤出机中挤出所需陶瓷坯体；
（3）烧结
将步骤（2）制得的陶瓷素坯放置于真空反应烧结炉中，在1750℃下烧结7h，制得碳化硅陶瓷；
（4）表面处理
将反应烧结碳化硅放置到高温炉中，以流量为20m3/h向高温炉中通入流动性的高纯氮气，加热温度为1300℃，保温时间为6h，获得表面氮化改性的反应烧结碳化硅陶瓷。
经检测，该实施例获得表面氮化改性的反应烧结碳化硅陶瓷的弯曲强度为379MPa，断裂韧性为3.24MPa·m1/2。
实施例3：一种表面氮化改性的反应烧结碳化硅陶瓷及其制备方法
表面氮化改性的反应烧结碳化硅陶瓷包括以下按重量份数计的原料：
碳化硅35份、炭黑7份、碳纤维7份、粘结剂5份、分散剂0.4份、去离子水40份；
所述粘结剂为羧甲基纤维素和PAF-Ⅱ型粉状粘结剂以1:1的重量比混合；所述分散剂为聚乙二醇和聚乙烯吡咯烷酮以1:1的重量比混合；所述碳化硅为F90的碳化硅、F120的碳化硅、F180的碳化硅和F1200的碳化硅以重量比为1:1:1:1的比例混合；所述炭黑和碳纤维的粒径分别为0.5μm和7μm。
上述表面氮化改性的反应烧结碳化硅陶瓷的制备方法，步骤如下：
（1）混料
取去离子水，将分散剂和粘结剂充分溶解，再称取F90的碳化硅、F120的碳化硅、F180的碳化硅、F1200的碳化硅、炭黑、碳纤维，在常温下利用滚筒混料机混料18h，将各组分混合均匀，获得混合物A；
（2）醒料
将步骤（1）所制得的混合物A放置到塑料膜内常温醒料20h，将醒好的混合物A放入挤出机中挤出所需陶瓷坯体；
（3）烧结
将步骤（2）制得的陶瓷素坯放置于真空反应烧结炉中，在1800℃下烧结5-12h，制得碳化硅陶瓷；
（4）表面处理
将反应烧结碳化硅放置到高温炉中，以流量为23m3/h向高温炉中通入流动性的高纯氮气，加热温度为1350℃，保温时间为4h，改性的反应烧结碳化硅陶瓷的弯曲强度为425MPa，断裂韧性为3.76MPa·m1/2。
Claims (8)
1.一种表面氮化改性的反应烧结碳化硅陶瓷，其特征在于，所述反应烧结碳化硅陶瓷包括以下按重量份数计的原料：
碳化硅5-40份、炭黑2-7份、碳纤维3-8份、粘结剂2-6份、分散剂0.1-0.4份、去离子水10-40份；
所述粘结剂为羧甲基纤维素和PAF-Ⅱ型粉状粘结剂以任意比混合；所述分散剂为聚乙二醇和聚乙烯吡咯烷酮以任意比混合。
2.根据权利要求1所述的反应烧结碳化硅陶瓷，其特征在于，所述碳化硅选自F90的碳化硅、F120的碳化硅、F180的碳化硅和F1200的碳化硅的混合物。
3.根据权利要求2所述的反应烧结碳化硅陶瓷，其特征在于，所述F90的碳化硅、F120的碳化硅、F180的碳化硅和F1200的碳化硅的重量比为1:2:1:2。
4.根据权利要求1所述的反应烧结碳化硅陶瓷，其特征在于，所述羧甲基纤维素和PAF-Ⅱ型粉状粘结剂以1:1的重量比混合。
5.根据权利要求1所述的反应烧结碳化硅陶瓷，其特征在于，所述聚乙二醇和聚乙烯吡咯烷酮以2:1的重量比混合。
6.根据权利要求1所述的反应烧结碳化硅陶瓷，其特征在于，所述炭黑和碳纤维的粒径分别为0.5-1μm和7-8μm。
7.如权利要求1-6任一项所述反应烧结碳化硅陶瓷的制备方法，步骤如下：
（1）混料
取去离子水，将分散剂和粘结剂充分溶解，再称取F90的碳化硅、F120的碳化硅、F180的碳化硅、F1200的碳化硅、炭黑、碳纤维，在常温下利用滚筒混料机混料8-20h，将各组分混合均匀，获得混合物A；
（2）醒料
将步骤（1）所制得的混合物A放置到塑料膜内常温醒料10-24h，将醒好的混合物A放入挤出机中挤出所需陶瓷坯体；
（3）烧结
将步骤（2）制得的陶瓷素坯放置于真空反应烧结炉中，在1500-1850℃下烧结5-12h，制得碳化硅陶瓷；
（4）表面处理
将反应烧结碳化硅放置到高温炉中，在加热同时通入流动的高纯氮气，进而生成表面氮化改性的反应烧结碳化硅陶瓷。
8.根据权利要求7所述的制备方法，其特征在于，所述步骤（4）中将反应烧结碳化硅放置到高温炉中，以流量为15-25m3/h向高温炉中通入流动性的高纯氮气，加热温度为1250-1350℃，保温时间为4-8h。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110669667.0A CN113307644A (zh) | 2021-06-17 | 2021-06-17 | 一种氮化改性反应烧结碳化硅陶瓷表面的方法 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110669667.0A CN113307644A (zh) | 2021-06-17 | 2021-06-17 | 一种氮化改性反应烧结碳化硅陶瓷表面的方法 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113307644A true CN113307644A (zh) | 2021-08-27 |
Family
ID=77379157
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110669667.0A Pending CN113307644A (zh) | 2021-06-17 | 2021-06-17 | 一种氮化改性反应烧结碳化硅陶瓷表面的方法 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113307644A (zh) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116573940A (zh) * | 2023-04-28 | 2023-08-11 | 合肥陶陶新材料科技有限公司 | 一种高韧性碳化硅陶瓷材料及其制备方法 |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3707083A1 (de) * | 1987-03-05 | 1988-09-15 | Laing Karsten | Verfahren zur herstellung von koerpern aus siliziumkarbid |
| CN101104559A (zh) * | 2007-07-24 | 2008-01-16 | 山东金鸿集团有限公司 | 一种碳纤维增强反应烧结碳化硅陶瓷及其制备方法 |
| CN101935218A (zh) * | 2010-09-03 | 2011-01-05 | 山东理工大学 | 挤出成型反应烧结碳化硅方梁的制备方法 |
| CN105712727A (zh) * | 2016-01-19 | 2016-06-29 | 山东宝纳新材料有限公司 | 一种高抗热震碳化硅复合陶瓷换热器管及其制备方法 |
| WO2019077318A1 (en) * | 2017-10-19 | 2019-04-25 | Vulcan Refractories Ltd | REFRACTORY MATERIAL |
| CN111747752A (zh) * | 2020-07-15 | 2020-10-09 | 山田研磨材料有限公司 | 一种表面改性的反应烧结碳化硅陶瓷及制备工艺 |
-
2021
- 2021-06-17 CN CN202110669667.0A patent/CN113307644A/zh active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3707083A1 (de) * | 1987-03-05 | 1988-09-15 | Laing Karsten | Verfahren zur herstellung von koerpern aus siliziumkarbid |
| CN101104559A (zh) * | 2007-07-24 | 2008-01-16 | 山东金鸿集团有限公司 | 一种碳纤维增强反应烧结碳化硅陶瓷及其制备方法 |
| CN101935218A (zh) * | 2010-09-03 | 2011-01-05 | 山东理工大学 | 挤出成型反应烧结碳化硅方梁的制备方法 |
| CN105712727A (zh) * | 2016-01-19 | 2016-06-29 | 山东宝纳新材料有限公司 | 一种高抗热震碳化硅复合陶瓷换热器管及其制备方法 |
| WO2019077318A1 (en) * | 2017-10-19 | 2019-04-25 | Vulcan Refractories Ltd | REFRACTORY MATERIAL |
| CN111747752A (zh) * | 2020-07-15 | 2020-10-09 | 山田研磨材料有限公司 | 一种表面改性的反应烧结碳化硅陶瓷及制备工艺 |
Non-Patent Citations (2)
| Title |
|---|
| 李双等: "炭黑含量对短纤维增强反应烧结碳化硅结构与性能的影响", 《稀有金属材料与工程》 * |
| 李钒等: "《冶金与材料近代物理化学研究方法》", 30 September 2018, 冶金工业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116573940A (zh) * | 2023-04-28 | 2023-08-11 | 合肥陶陶新材料科技有限公司 | 一种高韧性碳化硅陶瓷材料及其制备方法 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CA2178819A1 (en) | Low temperature, pressureless sintering of silicon nitride | |
| CN110590377A (zh) | 一种高β相致密氮化硅陶瓷及低温制备方法 | |
| CN112159232A (zh) | 一种高纯高致密碳化硅陶瓷及其制造方法 | |
| CN108439995B (zh) | 一种复相陶瓷及其制备方法 | |
| CN112409020B (zh) | 一种石墨材料表面耐高温抗氧化涂层及其制备方法 | |
| CN111533561A (zh) | 氮化硅基陶瓷球及其制备方法和应用 | |
| CN112142449A (zh) | 二维过渡金属碳化钛材料增强陶瓷复合材料及其制备方法 | |
| CN112028635A (zh) | 一种超高温陶瓷复合材料及制备方法 | |
| CN110627507B (zh) | 一种低温碳化硅陶瓷及其制备方法和应用 | |
| CN111470871A (zh) | 基于3d打印的低温共烧陶瓷超硬磨料聚合体的制备方法 | |
| CN101928148B (zh) | 一种基于硅烷偶联剂低温高致密碳化硅陶瓷制造方法 | |
| CN115536403A (zh) | 一种高韧氮化硅陶瓷材料及其制备方法 | |
| EP0322174B1 (en) | Process for making silicon nitride articles | |
| CN113307644A (zh) | 一种氮化改性反应烧结碳化硅陶瓷表面的方法 | |
| CN107746282A (zh) | 一种原位碳化硅纤维增强液相烧结碳化硅陶瓷及制造方法 | |
| CN106518119B (zh) | 一种致密的Ti2AlC/Al2O3纤维复合材料及其制备方法 | |
| CN110256093A (zh) | 一种降低熔渗工艺制备SiCf/SiC复合材料中残余硅含量的方法 | |
| CN101551012A (zh) | 含碳的碳化硅密封环及其制备方法 | |
| CN111517798A (zh) | 一种碳化物基陶瓷材料、制备方法及其应用 | |
| CN112341201A (zh) | 一种自结合碳化硅耐火材料及其制备方法 | |
| 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 | |
| CN114853489A (zh) | 低结合相含量的β-SiC结合SiC耐火材料及其制备方法与制品 | |
| CN109400176A (zh) | 一种高性能氮化硅陶瓷及其制备方法和应用 | |
| CN110526713B (zh) | 一种多孔碳化硅陶瓷及其制备方法和应用 | |
| CN114315364A (zh) | 一种先驱体加入纳米Si粉制备净SiC陶瓷的方法 |
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: 20210827 |