CN109095936A - 一种氮化硅陶瓷材料的增韧处理工艺 - Google Patents
一种氮化硅陶瓷材料的增韧处理工艺 Download PDFInfo
- Publication number
- CN109095936A CN109095936A CN201810951861.6A CN201810951861A CN109095936A CN 109095936 A CN109095936 A CN 109095936A CN 201810951861 A CN201810951861 A CN 201810951861A CN 109095936 A CN109095936 A CN 109095936A
- Authority
- CN
- China
- Prior art keywords
- weight
- parts
- silicon nitride
- carbon fiber
- treatment process
- 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.)
- Withdrawn
Links
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 24
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 16
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 13
- 230000008569 process Effects 0.000 title claims abstract description 12
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 28
- 239000004917 carbon fiber Substances 0.000 claims abstract description 28
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 28
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000005245 sintering Methods 0.000 claims abstract description 14
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 8
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 24
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 8
- 238000000498 ball milling Methods 0.000 claims description 8
- 229910002804 graphite Inorganic materials 0.000 claims description 8
- 239000010439 graphite Substances 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 229910052593 corundum Inorganic materials 0.000 claims description 7
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 6
- 238000011010 flushing procedure Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical class O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 4
- 239000000654 additive Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000002002 slurry Substances 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 230000000996 additive effect Effects 0.000 claims description 2
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 abstract description 15
- 239000007791 liquid phase Substances 0.000 abstract description 6
- 230000003026 anti-oxygenic effect Effects 0.000 abstract description 2
- 238000003181 co-melting Methods 0.000 abstract description 2
- 238000000280 densification Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 239000011241 protective layer Substances 0.000 abstract description 2
- 229910052814 silicon oxide Inorganic materials 0.000 abstract description 2
- 230000007704 transition Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 238000012545 processing Methods 0.000 description 4
- 239000012071 phase Substances 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000007822 coupling agent Substances 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- OKTJSMMVPCPJKN-YPZZEJLDSA-N carbon-10 atom Chemical group [10C] OKTJSMMVPCPJKN-YPZZEJLDSA-N 0.000 description 1
- OKTJSMMVPCPJKN-BJUDXGSMSA-N carbon-11 Chemical group [11C] OKTJSMMVPCPJKN-BJUDXGSMSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000004408 titanium dioxide Substances 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
- C04B35/58—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
- C04B35/584—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 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
- 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
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62844—Coating fibres
- C04B35/62847—Coating fibres with oxide ceramics
- C04B35/62849—Silica or silicates
-
- 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
- C04B35/62886—Coating the powders or the macroscopic reinforcing agents by wet chemical techniques
-
- 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
- C04B35/62892—Coating the powders or the macroscopic reinforcing agents with a coating layer consisting of particles
-
- 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
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—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
- C04B2235/65—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
- C04B2235/666—Applying a current during sintering, e.g. plasma sintering [SPS], electrical resistance heating or pulse electric current sintering [PECS]
-
- 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)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Ceramic Products (AREA)
Abstract
本发明公开了一种氮化硅陶瓷材料的增韧处理工艺，通过反应将二氧化硅包裹在碳纤维表面，与烧结助剂在高温下形成低温共融液相，一方面可以通过此液相完成液相烧结促进氮化硅陶瓷的致密化，使碳纤维更好的融合于氮化硅陶瓷中，提高陶瓷的断裂韧性；另一方面，二氧化硅发生玻璃态转变后，在碳纤维表面形成氧化硅保护层，提高了碳纤维的抗氧化性能，从而进一步起到了增强增韧的作用。
Description
技术领域
本发明属于陶瓷制备技术领域，具体涉及一种氮化硅陶瓷材料的增韧处理工艺。
背景技术
新型陶瓷作为一种新材料,其优异的性能和巨大的应用前景在材料领域中独树一帜,它们可以突破现有材料的应用限制,将成为继金属、高分子之后的第三种主要材料。伴随着航空航天、运载火箭的飞速发展，新型陶瓷得到了各行各业的关注，在很多领域得到了应用。
氮化硅（Si3N4）作为典型的强共价键结构材料，具有高硬度、高强度、耐腐蚀、耐磨损、抗氧化等独特的优良性能，在新型陶瓷中占有重要的地位.与其它材料比较, 氮化硅还具有比重小,热膨胀系数小,抗热冲击性好,自润性好等优势,是一类理想的结构陶瓷材料，其优异的性能和巨大的应用前景，激发了各方对它的兴趣和研究。然而，随着现代工业要求的不断提高，氮化硅陶瓷性能的进一步提升也势在必行。
发明内容
本发明的目的是提供一种氮化硅陶瓷材料的增韧处理工艺，以解决现有的氮化硅陶瓷性能韧性不足的问题。
本发明所要解决的技术问题采用以下的技术方案实现：
一种氮化硅陶瓷材料的增韧处理工艺，，包括以下步骤：
（1）将20-30重量份的碳纤维加入到100-200重量份的丙酮中，升温至 60-80℃，搅拌回流40-50h，过滤，用丙酮清洗2-5次，在真空干燥箱中干燥4-8h后将所得碳纤维加入到80-120重量份浓硝酸中，在60-90℃反应2-4h，过滤，用去离子水水洗至中性，干燥至恒重备用；
（2）将 20-30重量份1,4-对苯二异氰酸酯和3-5重量份甲苯，超声分散25-45min后，加入步骤（2）所得碳纤维及10-20重量份二月桂酸二丁基锡，30-50℃下搅拌反应4-7h，过滤，产物用无水甲苯反复冲洗2-5次，干燥至恒重备用；
（3）取40-60重量份纳米二氧化硅，加入 100-150重量份的1,4-二氧六环中进行超声分散1-3h后，加入步骤（2）所得碳纤维、5-10重量份三乙胺，30-50°C 下反应20-30h，过滤，产物用无水 1,4-二氧六环反复冲洗2-5次，干燥直至恒重；
（4）将85-100重量份的α相 Si3N4 粉、5-8份烧结助剂、步骤（3）所得物和300-400重量份乙醇放入滚筒式球磨机上球磨2-3h，将球磨后的浆料干燥1-2h后，研磨，过100-200目筛，备用；
（5）将步骤（4）所得物称重等分，装入石墨模具中，对模具预置 20-40MPa 的压力，并抽真空至 3-6Pa，然后开始通电升温，脉冲输出电压范围 2-12V，输出电流范围 0-5000A，在烧结至1300-1500℃后，升压至40-60MPa，5-10min后冷却即可。
进一步的，步骤（1）-（4）中所述干燥温度为30-60℃。
进一步的，步骤（4）所述烧结助剂为剂为Al2O3、 Y2O3混合物，其中质量比为Al2O3:Y2O3=1:1-2
进一步的，步骤（5）所述石墨模具直径为15-25mm。
本发明的有益效果为：对碳纤维进行酸处理后，碳纤维表面吸附大量的羟基，可与具有高反应活性的1,4-对苯二异氰酸酯偶联剂发生反应，加入分散后的二氧化硅，二氧化硅表面大量的硅羟基通过与偶联剂反应附着在碳纤维表面，形成二氧化硅包裹的碳纤维，将其与氮化硅粉末通过放点等离子烧结后，碳纤维表面的二氧化硅、与烧结助剂在高温下形成低温共融液相，一方面可以通过此液相完成液相烧结促进氮化硅陶瓷的致密化，使碳纤维更好的融合于氮化硅陶瓷中，提高陶瓷的断裂韧性；另一方面，二氧化硅发生玻璃态转变后，在碳纤维表面形成氧化硅保护层，提高了碳纤维的抗氧化性能，从而进一步起到了增强增韧的作用。
具体实施方式
实施例1
一种氮化硅陶瓷材料的增韧处理工艺，其特征在于，包括以下步骤：
（1）将25重量份的碳纤维加入到150重量份的丙酮中，升温至 60℃，搅拌回流45h，过滤，用丙酮清洗3次，在真空干燥箱中干燥5h后将所得碳纤维加入到100重量份浓硝酸中，在80℃反应3h，过滤，用去离子水水洗至中性，干燥至恒重备用；
（2）将 25重量份1,4-对苯二异氰酸酯和5重量份甲苯，超声分散30min后，加入步骤（2）所得碳纤维及10重量份二月桂酸二丁基锡，45℃下搅拌反应5h，过滤，产物用无水甲苯反复冲洗3次，干燥至恒重备用；
（3）取50重量份纳米二氧化硅，加入 130重量份的1,4-二氧六环中进行超声分散2h后，加入步骤（2）所得碳纤维、5重量份三乙胺，40℃ 下反应20h，过滤，产物用无水 1,4-二氧六环反复冲洗3次，干燥直至恒重；
（4）将90重量份的α相 Si3N4 粉、7份烧结助剂、步骤（3）所得物和300重量份乙醇放入滚筒式球磨机上球磨2h，将球磨后的浆料干燥1h后，研磨，过100目筛，备用；
（5）将步骤（4）所得物称重等分，装入石墨模具中，对模具预置 30MPa 的压力，并抽真空至5Pa，然后开始通电升温，脉冲输出电压范围 2-12V，输出电流范围 0-5000A，在烧结至1500℃后，升压至50MPa，8min后冷却即可。
进一步的，步骤（1）-（4）中所述干燥温度为45℃。
进一步的，步骤（4）所述烧结助剂为Al2O3、 Y2O3混合物，其中质量比为Al2O3: Y2O3=1:1。
进一步的，步骤（5）所述石墨模具直径为20mm。
实施例2
（1）将27重量份的碳纤维加入到160重量份的丙酮中，升温至 65℃，搅拌回流46h，过滤，用丙酮清洗3次，在真空干燥箱中干燥5h后将所得碳纤维加入到105重量份浓硝酸中，在75℃反应3.5h，过滤，用去离子水水洗至中性，干燥至恒重备用；
（2）将 28重量份1,4-对苯二异氰酸酯和6重量份甲苯，超声分散35min后，加入步骤（2）所得碳纤维及11重量份二月桂酸二丁基锡，46℃下搅拌反应5h，过滤，产物用无水甲苯反复冲洗3次，干燥至恒重备用；
（3）取55重量份纳米二氧化硅，加入 120重量份的1,4-二氧六环中进行超声分散3h后，加入步骤（2）所得碳纤维、6重量份三乙胺，45℃ 下反应22h，过滤，产物用无水 1,4-二氧六环反复冲洗3次，干燥直至恒重；
（4）将95重量份的α相 Si3N4 粉、7份烧结助剂、步骤（3）所得物和290重量份乙醇放入滚筒式球磨机上球磨2.5h，将球磨后的浆料干燥1h后，研磨，过150目筛，备用；
（5）将步骤（4）所得物称重等分，装入石墨模具中，对模具预置 32MPa 的压力，并抽真空至6Pa，然后开始通电升温，脉冲输出电压范围 2-12V，输出电流范围 0-5000A，在烧结至1550℃后，升压至50MPa，10min后冷却即可。
进一步的，步骤（1）-（4）中所述干燥温度为50℃。
进一步的，步骤（4）所述烧结助剂为Al2O3、 Y2O3混合物，其中质量比为Al2O3: Y2O3=1:2。
进一步的，步骤（5）所述石墨模具直径为22mm。
对比实施例1
本对比实施例1与实施例1相比，省去步骤（1）的处理操作，除此外的方法步骤均相同。
对比实施例2
本对比实施例1与实施例1相比，省去步骤（1）、步骤（2）的处理操作，除此外的方法步骤均相同。
对比实施例3
本对比实施例2与实施例1相比，省去步骤（3）的处理操作，除此外的方法步骤均相同。
对照组
氮化硅陶瓷
根据以上实施例、对比实施例的实验条件，制备出不同的陶瓷，完成后对各组产品的断裂韧性进行测试，具体对比数据如下表1所示：
表1
由上表1可以看出，本发明提供的氮化硅陶瓷材料的增韧处理工艺，提升了氮化硅陶瓷的抗弯性能和断裂韧性，具有很好的推广价值。
Claims (4)
1.一种氮化硅陶瓷材料的增韧处理工艺，其特征在于，包括以下步骤：
（1）将20-30重量份的碳纤维加入到100-200重量份的丙酮中，升温至 60-80℃，搅拌回流40-50h，过滤，用丙酮清洗2-5次，在真空干燥箱中干燥4-8h后将所得碳纤维加入到80-120重量份浓硝酸中，在60-90℃反应2-4h，过滤，用去离子水水洗至中性，干燥至恒重备用；
（2）将 20-30重量份1,4-对苯二异氰酸酯和3-5重量份甲苯，超声分散25-45min后，加入步骤（2）所得碳纤维及10-20重量份二月桂酸二丁基锡，30-50℃下搅拌反应4-7h，过滤，产物用无水甲苯反复冲洗2-5次，干燥至恒重备用；
（3）取40-60重量份纳米二氧化硅，加入 100-150重量份的1,4-二氧六环中进行超声分散1-3h后，加入步骤（2）所得碳纤维、5-10重量份三乙胺，30-50°C 下反应20-30h，过滤，产物用无水 1,4-二氧六环反复冲洗2-5次，干燥直至恒重；
（4）将85-100重量份的α相 Si3N4粉、5-8份烧结助剂、步骤（3）所得物和300-400重量份乙醇放入滚筒式球磨机上球磨2-3h，将球磨后的浆料干燥1-2h后，研磨，过100-200目筛，备用；
（5）将步骤（4）所得物称重等分，装入石墨模具中，对模具预置 20-40MPa 的压力，并抽真空至 3-6Pa，然后开始通电升温，脉冲输出电压范围 2-12V，输出电流范围 0-5000A，在烧结至1300-1500℃后，升压至40-60MPa，5-10min后冷却即可。
2.根据权利要求1所述的一种氮化硅陶瓷材料的增韧处理工艺，其特征在于，步骤（1）-（4）中所述干燥温度为30-60℃。
3. 根据权利要求1所述的一种氮化硅陶瓷材料的增韧处理工艺，其特征在于，步骤（4）所述烧结助剂为Al2O3、 Y2O3混合物，其中质量比为Al2O3:Y2O3=1:1-2。
4.根据权利要求1所述的一种氮化硅陶瓷材料的增韧处理工艺，其特征在于，步骤（5）所述石墨模具直径为15-25mm。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810951861.6A CN109095936A (zh) | 2018-08-21 | 2018-08-21 | 一种氮化硅陶瓷材料的增韧处理工艺 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810951861.6A CN109095936A (zh) | 2018-08-21 | 2018-08-21 | 一种氮化硅陶瓷材料的增韧处理工艺 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109095936A true CN109095936A (zh) | 2018-12-28 |
Family
ID=64850396
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810951861.6A Withdrawn CN109095936A (zh) | 2018-08-21 | 2018-08-21 | 一种氮化硅陶瓷材料的增韧处理工艺 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109095936A (zh) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114477919A (zh) * | 2022-03-08 | 2022-05-13 | 彭材大 | 一种抗渗再生混凝土及其制备方法 |
| CN116924819A (zh) * | 2023-07-19 | 2023-10-24 | 哈尔滨工业大学 | 一种SiBCN复合材料及其制备方法 |
| CN118125852A (zh) * | 2024-05-08 | 2024-06-04 | 杭州幄肯新材料科技有限公司 | 一种增强预制体碳碳复合材料及其制备方法 |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57206596A (en) * | 1981-06-11 | 1982-12-17 | Chobe Taguchi | Backing strip material for welding |
| JPS61197472A (ja) * | 1985-02-27 | 1986-09-01 | 工業技術院長 | 炭化ケイ素繊維強化炭化ケイ素複合体の製造方法 |
| US4956317A (en) * | 1987-12-01 | 1990-09-11 | Ngk Spark Plug Co., Ltd. | Whisker-reinforced ceramics |
| US20050181192A1 (en) * | 2001-01-16 | 2005-08-18 | Steffier Wayne S. | Fiber-reinforced ceramic composite material comprising a matrix with a nanolayered microstructure |
| CN103910532A (zh) * | 2013-01-05 | 2014-07-09 | 中国科学院宁波材料技术与工程研究所 | 涂层无机纤维增韧max相陶瓷复合材料、其制备方法及用途 |
| CN104609865A (zh) * | 2015-02-09 | 2015-05-13 | 广东工业大学 | 一种氮化硅基导电陶瓷的制备方法及氮化硅基导电陶瓷刀具的成型方法 |
| CN105272326A (zh) * | 2015-11-23 | 2016-01-27 | 哈尔滨工业大学 | 一种碳纳米管改性碳纤维增强SiBCN陶瓷复合材料的制备方法及应用 |
-
2018
- 2018-08-21 CN CN201810951861.6A patent/CN109095936A/zh not_active Withdrawn
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57206596A (en) * | 1981-06-11 | 1982-12-17 | Chobe Taguchi | Backing strip material for welding |
| JPS61197472A (ja) * | 1985-02-27 | 1986-09-01 | 工業技術院長 | 炭化ケイ素繊維強化炭化ケイ素複合体の製造方法 |
| US4956317A (en) * | 1987-12-01 | 1990-09-11 | Ngk Spark Plug Co., Ltd. | Whisker-reinforced ceramics |
| US20050181192A1 (en) * | 2001-01-16 | 2005-08-18 | Steffier Wayne S. | Fiber-reinforced ceramic composite material comprising a matrix with a nanolayered microstructure |
| US20050233127A1 (en) * | 2001-01-16 | 2005-10-20 | Steffier Wayne S | Fiber-reinforced ceramic composite material comprising a matrix with a nanolayered microstructure |
| CN103910532A (zh) * | 2013-01-05 | 2014-07-09 | 中国科学院宁波材料技术与工程研究所 | 涂层无机纤维增韧max相陶瓷复合材料、其制备方法及用途 |
| CN104609865A (zh) * | 2015-02-09 | 2015-05-13 | 广东工业大学 | 一种氮化硅基导电陶瓷的制备方法及氮化硅基导电陶瓷刀具的成型方法 |
| CN105272326A (zh) * | 2015-11-23 | 2016-01-27 | 哈尔滨工业大学 | 一种碳纳米管改性碳纤维增强SiBCN陶瓷复合材料的制备方法及应用 |
Non-Patent Citations (2)
| Title |
|---|
| G. LOGESH ET AL.: "Mechanical and dielectric properties of carbon fiber reinforced reaction bonded silicon nitride composites", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
| 豆鹏飞: "碳材料增韧氮化硅陶瓷研究进展", 《陶瓷》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114477919A (zh) * | 2022-03-08 | 2022-05-13 | 彭材大 | 一种抗渗再生混凝土及其制备方法 |
| CN116924819A (zh) * | 2023-07-19 | 2023-10-24 | 哈尔滨工业大学 | 一种SiBCN复合材料及其制备方法 |
| CN118125852A (zh) * | 2024-05-08 | 2024-06-04 | 杭州幄肯新材料科技有限公司 | 一种增强预制体碳碳复合材料及其制备方法 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107778019B (zh) | 一种制备碳化硅晶须补强增韧陶瓷基复合材料的方法 | |
| CN100445235C (zh) | 一种氮化铝增强碳化硅陶瓷及其制备方法 | |
| CN109095936A (zh) | 一种氮化硅陶瓷材料的增韧处理工艺 | |
| CN104045350B (zh) | 一种采用反应烧结工艺制备氮化硅-碳化硅复合陶瓷材料的方法 | |
| CN106966732B (zh) | 一种细粉碳化硅陶瓷及其制备方法 | |
| CN106297904B (zh) | UO2‑SiC燃料芯块的制备方法及采用该制备方法制成的UO2‑SiC燃料芯块 | |
| CN101555143A (zh) | 常压烧结碳化硅陶瓷的制备方法 | |
| CN103553632B (zh) | 一种致密化氮化硅陶瓷材料的制备方法 | |
| CN103834988A (zh) | 一种制备纳米碳化硅晶须的方法 | |
| CN109467438A (zh) | 一种碳化硅陶瓷光固化成型方法 | |
| CN100506694C (zh) | 一种用稻壳制备电子级球形硅微粉的方法 | |
| CN102176436A (zh) | 高性能Diamond/SiC电子封装材料的制备工艺 | |
| CN106083068A (zh) | 一种水基造粒并直接冷等静压成型的氮化硅陶瓷的制备方法 | |
| CN114956828A (zh) | 碳化硅陶瓷及其制备方法和应用 | |
| CN107935576B (zh) | 氮化硅结合莫来石-碳化硅陶瓷复合材料及其制备方法 | |
| CN112159234A (zh) | 一种高熵陶瓷粉体及其制备方法和应用 | |
| CN103482873A (zh) | 振动注浆成型方法制备熔融石英陶瓷 | |
| CN101734925B (zh) | 可控气孔率的氮化硅多孔陶瓷及制备方法 | |
| CN103820691A (zh) | 一种FeAl/TiC复合材料的常压烧结制备方法 | |
| CN106927801B (zh) | 用于石英陶瓷制备的功能化熔融石英粉的制备方法及功能化熔融石英粉 | |
| CN102267814A (zh) | 高孔隙率磷酸盐结合氮化硅多孔陶瓷的制备方法 | |
| CN103342547A (zh) | 一种制备高致密度熔融石英陶瓷的方法 | |
| CN114180980A (zh) | 一种自增韧99氧化铝陶瓷基板及其制备方法 | |
| CN107226700A (zh) | 一种Si3N4‑BN‑MAS陶瓷复合材料及其制备方法 | |
| CN107793138B (zh) | 一种氧化铝陶瓷 |
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 | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20181228 |
|
| WW01 | Invention patent application withdrawn after publication |