CN118637920A - A preparation method of gel casting pressureless sintered silicon carbide ceramics - Google Patents
A preparation method of gel casting pressureless sintered silicon carbide ceramics Download PDFInfo
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 115
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 106
- 239000000919 ceramic Substances 0.000 title claims abstract description 85
- 238000002360 preparation method Methods 0.000 title claims abstract description 44
- 238000005266 casting Methods 0.000 title description 5
- 239000000843 powder Substances 0.000 claims abstract description 101
- 238000003756 stirring Methods 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000008367 deionised water Substances 0.000 claims abstract description 26
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 26
- 238000001746 injection moulding Methods 0.000 claims abstract description 24
- 239000002002 slurry Substances 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 239000002270 dispersing agent Substances 0.000 claims abstract description 12
- 239000000375 suspending agent Substances 0.000 claims abstract description 11
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 9
- 239000000178 monomer Substances 0.000 claims abstract description 9
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 239000003999 initiator Substances 0.000 claims abstract description 8
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 238000007873 sieving Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 29
- 239000000047 product Substances 0.000 claims description 26
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 18
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 17
- 229920006322 acrylamide copolymer Polymers 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 13
- -1 dimethyl allyl ammonium chloride-acrylamide Chemical compound 0.000 claims description 11
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- 239000006229 carbon black Substances 0.000 claims description 9
- 239000002244 precipitate Substances 0.000 claims description 8
- 238000001272 pressureless sintering Methods 0.000 claims description 8
- 238000002347 injection Methods 0.000 claims description 7
- 239000007924 injection Substances 0.000 claims description 7
- 229910052582 BN Inorganic materials 0.000 claims description 6
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 5
- 239000002518 antifoaming agent Substances 0.000 claims description 2
- 238000005245 sintering Methods 0.000 abstract description 10
- 239000013530 defoamer Substances 0.000 abstract description 6
- 239000000203 mixture Substances 0.000 description 17
- 230000000694 effects Effects 0.000 description 10
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- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 3
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- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 description 2
- 125000003368 amide group Chemical group 0.000 description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 2
- YIOJGTBNHQAVBO-UHFFFAOYSA-N dimethyl-bis(prop-2-enyl)azanium Chemical compound C=CC[N+](C)(C)CC=C YIOJGTBNHQAVBO-UHFFFAOYSA-N 0.000 description 2
- ZWIBGKZDAWNIFC-UHFFFAOYSA-N disuccinimidyl suberate Chemical compound O=C1CCC(=O)N1OC(=O)CCCCCCC(=O)ON1C(=O)CCC1=O ZWIBGKZDAWNIFC-UHFFFAOYSA-N 0.000 description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 2
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- FJWSMXKFXFFEPV-UHFFFAOYSA-N prop-2-enamide;hydrochloride Chemical compound Cl.NC(=O)C=C FJWSMXKFXFFEPV-UHFFFAOYSA-N 0.000 description 2
- 125000001453 quaternary ammonium group Chemical group 0.000 description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 2
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- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 1
- 150000003863 ammonium salts Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 229920006158 high molecular weight polymer Polymers 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
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- 238000004381 surface treatment Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
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Abstract
本申请涉及一种凝胶注成型无压烧结碳化硅陶瓷的制备方法,包括如下步骤:制备组分A:将单体、交联剂、去离子水、分散剂、悬浮剂,以及一部分陶瓷粉体混合,搅拌,搅拌后干燥,过筛打粉后得到组分A;制备组分B:将消泡剂、催化剂、引发剂与剩余的陶瓷粉体混合,搅拌,搅拌后干燥,过筛打粉得到组分B;碳化硅陶瓷制备:将组分A与组分B混合后,加入去离子水混合形成浆料整体,固化后得到坯体,将坯体干燥,干燥后的坯体在2100‑2200℃的温度范围进行无压烧结,保温2‑5h,得到碳化硅陶瓷产品;单体包括丙烯酰胺,交联剂包括亚甲基双丙烯酰胺。本申请在制备碳化硅陶瓷产品时,有效提升碳化硅陶瓷制备时的可控性,且绿色环保,产品质量大幅提升。The present application relates to a preparation method of a gel injection molding pressureless sintered silicon carbide ceramic, comprising the following steps: preparing component A: mixing monomer, cross-linking agent, deionized water, dispersant, suspending agent, and a portion of ceramic powder, stirring, drying after stirring, sieving and powdering to obtain component A; preparing component B: mixing defoamer, catalyst, initiator with the remaining ceramic powder, stirring, drying after stirring, sieving and powdering to obtain component B; preparing silicon carbide ceramics: after mixing component A with component B, adding deionized water to mix to form a slurry as a whole, curing to obtain a green body, drying the green body, and sintering the dried green body without pressure at a temperature range of 2100-2200°C, keeping warm for 2-5h, and obtaining a silicon carbide ceramic product; the monomer includes acrylamide, and the cross-linking agent includes methylene bisacrylamide. When preparing silicon carbide ceramic products, the present application effectively improves the controllability of silicon carbide ceramics during preparation, and is green and environmentally friendly, and the product quality is greatly improved.
Description
技术领域Technical Field
本申请涉及陶瓷制备技术的领域,尤其是涉及一种凝胶注成型无压烧结碳化硅陶瓷的制备方法。The present application relates to the field of ceramic preparation technology, and in particular to a method for preparing gel-casting pressureless sintered silicon carbide ceramics.
背景技术Background Art
碳化硅陶瓷具有优良的常温力学性能,抗弯强度、抗氧化性、耐腐蚀性、耐磨性能等,也具有良好的高温力学性能。陶瓷制备可以采用热压烧结、无压烧结、热等静压烧结等,高温强度能够一直维持到1600℃。今年来随着碳化硅制品烧结理论的发展,微粉性能的提高,烧结助剂的多样化和深入研究等,采用无压烧结工艺烧结高性能碳化硅制品的工艺开始发展完善,且生产成本较低,对产品的形状尺寸没有限制。Silicon carbide ceramics have excellent room temperature mechanical properties, bending strength, oxidation resistance, corrosion resistance, wear resistance, etc., and also have good high temperature mechanical properties. Ceramic preparation can be done by hot pressing sintering, pressureless sintering, hot isostatic pressing sintering, etc., and the high temperature strength can be maintained up to 1600°C. This year, with the development of sintering theory of silicon carbide products, the improvement of micro powder performance, the diversification and in-depth research of sintering aids, the process of sintering high-performance silicon carbide products using pressureless sintering has begun to develop and improve, and the production cost is low, and there is no restriction on the shape and size of the product.
近年来,新的胶态成型如压滤成型、凝胶注模成型及直接凝固注模成型等等原位固化是制备高可靠性、复杂形状的陶瓷部件的有效方法,凝胶注模成型在多孔材料、复合材料、功能材料领域已经得到广泛研究,但是凝胶注固化后的坯体不能利用、陶瓷胶料的多少根据所成型的制品和体积进行计算,对于大尺寸的产品,固化整体发热较大,固化可控性能较低,成功率较低。In recent years, new colloidal molding such as filter press molding, gel injection molding and direct solidification injection molding, etc., in-situ curing is an effective method for preparing high-reliability, complex-shaped ceramic parts. Gel injection molding has been widely studied in the fields of porous materials, composite materials, and functional materials. However, the green body after gel injection curing cannot be used, and the amount of ceramic glue is calculated according to the molded product and volume. For large-sized products, the overall heat generation during curing is large, the curing controllability is low, and the success rate is low.
发明内容Summary of the invention
为了解决上述技术问题,本申请提供一种凝胶注成型无压烧结碳化硅陶瓷的制备方法。In order to solve the above technical problems, the present application provides a method for preparing gel-casting pressureless sintered silicon carbide ceramics.
本申请提供的一种凝胶注无压烧结碳化硅陶瓷的制备方法采用如下的技术方案:The present application provides a method for preparing a gel-injection pressureless sintered silicon carbide ceramic using the following technical solution:
一种凝胶注成型无压烧结碳化硅陶瓷的制备方法,包括如下步骤:A method for preparing a gel-casting pressureless sintered silicon carbide ceramic comprises the following steps:
制备组分A:将单体、交联剂、去离子水、分散剂、悬浮剂,以及一部分陶瓷粉体混合,搅拌,搅拌后干燥,过筛打粉后得到组分A;Preparation of component A: Mixing monomers, crosslinking agents, deionized water, dispersants, suspending agents, and a portion of ceramic powder, stirring, drying after stirring, and sieving and powdering to obtain component A;
制备组分B:将消泡剂、催化剂、引发剂与剩余的陶瓷粉体混合,搅拌,搅拌后干燥,过筛打粉得到组分B;Preparation of component B: mixing the defoamer, catalyst, initiator and remaining ceramic powder, stirring, drying after stirring, sieving and powdering to obtain component B;
碳化硅陶瓷制备:将组分A与组分B混合后,加入去离子水混合形成浆料整体,固化后得到坯体,将坯体干燥,干燥后的坯体在2100-2200℃的温度范围进行无压烧结,保温2-5h,得到碳化硅陶瓷产品;Preparation of silicon carbide ceramics: After mixing component A and component B, add deionized water to form a slurry as a whole, solidify to obtain a green body, dry the green body, and perform pressureless sintering at a temperature range of 2100-2200°C for 2-5 hours to obtain a silicon carbide ceramic product;
所述单体包括丙烯酰胺,所述交联剂包括亚甲基双丙烯酰胺。The monomer includes acrylamide, and the cross-linking agent includes methylene bisacrylamide.
通过采用上述技术方案,分别配置组分A与组分B,当组分A与组分B相遇时才能够开始固化,对于大尺寸产品制备能够更好的控制,并且组分A与组分B未接触的部分能够进行保留,在下次进行制备时再次使用,更加节能环保,降低了生产成本。By adopting the above technical solution, component A and component B are configured separately, and solidification can only begin when component A meets component B. The preparation of large-size products can be better controlled, and the parts of component A and component B that are not in contact can be retained and reused in the next preparation, which is more energy-saving and environmentally friendly and reduces production costs.
作为优选,所述步骤制备组分A与步骤制备组分B中,搅拌时的搅拌温度均为5-10℃,搅拌速度均为100-150r/min。Preferably, in the step of preparing component A and the step of preparing component B, the stirring temperature is 5-10° C. and the stirring speed is 100-150 r/min.
通过采用上述技术方案,控制组分A与组分B接触时的搅拌温度与搅拌速度在上述限定范围内,能够进一步提升制备得到的浆料的稳定性,低温高速搅拌时,能够抑制单体与交联剂发生交联固化反应并使得组分A与组分B接触更加充分,从而便于后续对得到的浆料进行控制。By adopting the above technical solution, the stirring temperature and stirring speed when component A and component B are in contact are controlled within the above-mentioned limited range, which can further improve the stability of the prepared slurry. When stirring at low temperature and high speed, the cross-linking and curing reaction between the monomer and the cross-linking agent can be suppressed and the contact between component A and component B can be more sufficient, thereby facilitating the subsequent control of the obtained slurry.
作为优选,所述分散剂占浆料整体的2-5%,所述悬浮剂占浆料整体的0.4-0.6%。Preferably, the dispersant accounts for 2-5% of the total slurry, and the suspending agent accounts for 0.4-0.6% of the total slurry.
通过采用上述技术方案,优选分散剂与悬浮剂的含量在上述范围之内,能够进一步提升整体浆料中各个组份之间的均匀性与稳定性,对于制备得到的碳化硅陶瓷产品质量也有所改善。By adopting the above technical solution, preferably the content of the dispersant and the suspending agent is within the above range, which can further improve the uniformity and stability of the various components in the overall slurry, and also improve the quality of the prepared silicon carbide ceramic product.
作为优选,所述步骤碳化硅陶瓷制备中组分A与组分B之间的质量比为(3.8-4.2):1。Preferably, the mass ratio between component A and component B in the preparation of silicon carbide ceramic in the step is (3.8-4.2):1.
作为优选,所述陶瓷粉体包括碳化硅表面改性超细粉、炭黑与氮化硼,所述碳化硅表面改性超细粉、炭黑与氮化硼之间的质量比为(97.2-97.6):2:0.6。Preferably, the ceramic powder comprises silicon carbide surface modified ultrafine powder, carbon black and boron nitride, and the mass ratio of the silicon carbide surface modified ultrafine powder, carbon black and boron nitride is (97.2-97.6):2:0.6.
通过采用上述技术方案,使用碳化硅表面改性超细粉、炭黑与氮化硼混合制备得到陶瓷粉体,使得陶瓷粉体的综合性能得到提升,控制碳化硅超细粉、炭黑与氮化硼之间的质量比在上述范围之内,能够进一步提升陶瓷粉体制备得到的产品的质量。By adopting the above technical scheme, ceramic powder is prepared by mixing silicon carbide surface modified ultrafine powder, carbon black and boron nitride, so that the comprehensive performance of the ceramic powder is improved. By controlling the mass ratio of silicon carbide ultrafine powder, carbon black and boron nitride within the above range, the quality of the product prepared from the ceramic powder can be further improved.
作为优选,所述碳化硅表面改性超细粉采用如下方法制备而成:Preferably, the silicon carbide surface modified ultrafine powder is prepared by the following method:
将碳化硅超细粉与去离子水混合后,加入改性剂与表面活性剂,搅拌反应后离心,将沉淀物洗涤后干燥,得到碳化硅表面改性超细粉。After mixing the silicon carbide ultrafine powder with deionized water, adding a modifier and a surfactant, stirring for reaction and then centrifuging, washing and drying the precipitate, and obtaining the silicon carbide surface modified ultrafine powder.
通过采用上述技术方案,使用改性剂与表面活性剂对碳化硅超细粉进行处理后,能够有效提升碳化硅超细粉的在体系中的分散效果,同时能够使得制备得到的浆料具有良好的流变性和沉降稳定性,同时能够提升浆料固含量,进一步提升了制备得到的碳化硅陶瓷的产品质量。By adopting the above technical scheme, after using modifiers and surfactants to treat silicon carbide ultrafine powder, the dispersion effect of silicon carbide ultrafine powder in the system can be effectively improved, and the prepared slurry can have good rheological properties and sedimentation stability. At the same time, the solid content of the slurry can be increased, and the product quality of the prepared silicon carbide ceramics can be further improved.
作为优选,所述改性剂、表面活性剂与碳化硅表面改性超细粉之间的质量比为(0.49-0.51):1:19.8。Preferably, the mass ratio of the modifier, surfactant and silicon carbide surface modified ultrafine powder is (0.49-0.51):1:19.8.
通过采用上述技术方案,优选改性剂、表面活性剂与碳化硅表面改性超细粉之间的质量比在上述范围之内,能够进一步提升碳化硅超细粉改性后的综合性能。By adopting the above technical solution, the mass ratio of the modifier, the surfactant and the surface-modified silicon carbide ultrafine powder is preferably within the above range, which can further improve the comprehensive performance of the modified silicon carbide ultrafine powder.
作为优选,所述改性剂包括二甲基而烯丙基氯化铵-丙烯酰胺共聚物。Preferably, the modifier comprises dimethyl allyl ammonium chloride-acrylamide copolymer.
通过采用上述技术方案,二甲基二烯丙基氯化铵-丙烯酰胺共聚物是一种聚季铵盐物质,其分子链中含有大量的酰胺基和季铵基,季铵基团具有正电荷,与碳化硅超细粉体表面能够形成高亲和力吸附,亲水性的酰胺基团可以延伸至水中,从而使得改性后的碳化硅超细粉体颗粒具有良好的亲水性与空间位阻,进而使得碳化硅超细粉体颗粒的分散性得到提升,以提升制备得到的碳化硅陶瓷的产品质量。By adopting the above technical scheme, the dimethyldiallylammonium chloride-acrylamide copolymer is a polyquaternary ammonium salt substance, and its molecular chain contains a large number of amide groups and quaternary ammonium groups. The quaternary ammonium groups have a positive charge and can form high-affinity adsorption with the surface of silicon carbide ultrafine powder. The hydrophilic amide groups can extend into water, so that the modified silicon carbide ultrafine powder particles have good hydrophilicity and steric hindrance, thereby improving the dispersibility of the silicon carbide ultrafine powder particles, thereby improving the product quality of the prepared silicon carbide ceramics.
作为优选,所述表面活性剂包括月桂醇硫酸钠。Preferably, the surfactant comprises sodium lauryl sulfate.
通过采用上述技术方案,以月桂醇硫酸钠作为表面活性剂添加后,月桂醇硫酸钠中的硫酸根能够吸附在碳化硅超细粉体的表面,在改性剂提升碳化硅超细粉体的分散性的同时,月桂醇硫酸钠能够自发地富集在碳化硅超细粉体的表面,从而提升了碳化硅超细粉体的稳定性,进一步提升了制备得到的碳化硅陶瓷的产品质量。By adopting the above technical scheme, after sodium lauryl sulfate is added as a surfactant, the sulfate ions in the sodium lauryl sulfate can be adsorbed on the surface of the silicon carbide ultrafine powder. While the modifier improves the dispersibility of the silicon carbide ultrafine powder, the sodium lauryl sulfate can spontaneously enrich on the surface of the silicon carbide ultrafine powder, thereby improving the stability of the silicon carbide ultrafine powder and further improving the product quality of the prepared silicon carbide ceramics.
作为优选,所述搅拌反应时反应温度为88-92℃。Preferably, the reaction temperature during the stirring reaction is 88-92°C.
通过采用上述技术方案,优选搅拌反应时的反应温度在上述范围内,能够更好地促进改性剂、表面活性剂与碳化硅超细粉体之间的结合,从而提升了制备得到的碳化硅超细粉体的整体的分散性能与质量。By adopting the above technical solution, the reaction temperature during the stirring reaction is preferably within the above range, which can better promote the combination of the modifier, surfactant and silicon carbide ultrafine powder, thereby improving the overall dispersion performance and quality of the prepared silicon carbide ultrafine powder.
综上所述,本申请包括以下至少一种有益技术效果:In summary, the present application includes at least one of the following beneficial technical effects:
分别制备组分A与组分B,当组分A与组分B组分相遇时,才进行固化,对于大尺寸的碳化硅陶瓷制备可控性有所提升,同时制备过程中,组分A与组分B未接触到一起的部分能够进行回收,并用在后续的碳化硅陶瓷产品制备中,绿色环保,生产成本有所降低;Component A and component B are prepared separately. When component A and component B meet, they are solidified. The controllability of large-sized silicon carbide ceramic preparation is improved. At the same time, during the preparation process, the parts of component A and component B that are not in contact with each other can be recycled and used in the subsequent preparation of silicon carbide ceramic products. It is green and environmentally friendly, and the production cost is reduced.
使用改性剂与表面活性剂对碳化硅超细粉体进行表面处理后,能够有效提升碳化硅陶瓷粉体整体的分散性,使得陶瓷粉体能够在浆料中分散更加均匀,制备的坯体能够更加稳定,且有效提升了坯体的固含量,减少了坯体坍塌等现象,后续制备得到的碳化硅陶瓷产品的质量能够有效提升。After surface treatment of silicon carbide ultrafine powder with modifiers and surfactants, the overall dispersibility of silicon carbide ceramic powder can be effectively improved, so that the ceramic powder can be dispersed more evenly in the slurry, the prepared green body can be more stable, and the solid content of the green body can be effectively increased, reducing the collapse of the green body and other phenomena. The quality of the silicon carbide ceramic products prepared subsequently can be effectively improved.
具体实施方式DETAILED DESCRIPTION
本申请实施例公开一种凝胶注成型无压烧结碳化硅陶瓷的制备方法,以下结合实施例对本申请作进一步详细说明:The present application discloses a method for preparing a gel-cast pressureless sintered silicon carbide ceramic. The present application is further described in detail below in conjunction with the examples:
原料准备:Raw material preparation:
单体:丙烯酰胺(CAS号:79-06-1);交联剂:亚甲基双丙烯酰胺(CAS号:110-26-9);分散剂:分散剂为DolaPIX CE 64与MQ-5088以质量比为1:1混合得到而成;悬浮剂:MQ-818;消泡剂:正辛醇(CAS号:111-87-5);催化剂:四甲基乙二胺(CAS号:110-18-9);引发剂:由质量分数为5%的过硫酸铵,其余为去离子水混合配置得到。Monomer: acrylamide (CAS No.: 79-06-1); cross-linking agent: methylene bisacrylamide (CAS No.: 110-26-9); dispersant: the dispersant is prepared by mixing DolaPIX CE 64 and MQ-5088 in a mass ratio of 1:1; suspending agent: MQ-818; defoaming agent: n-octanol (CAS No.: 111-87-5); catalyst: tetramethylethylenediamine (CAS No.: 110-18-9); initiator: prepared by mixing 5% by mass of ammonium persulfate and the rest of deionized water.
凝胶注成型制备无压烧结碳化硅陶瓷的方法:Method for preparing pressureless sintered silicon carbide ceramics by gel casting:
制备组分A:将单体、交联剂、去离子水、分散剂、悬浮剂以及一部分陶瓷粉体混合,在5-10℃的温度下,以100-150r/min的速度搅拌1.5-2.5h,随后转移至真空干燥箱中以35-45℃的温度条件干燥24h,过筛后打粉,得到组分A。Preparation of component A: Mix the monomer, cross-linking agent, deionized water, dispersant, suspending agent and a portion of ceramic powder, stir at 100-150 r/min for 1.5-2.5 h at a temperature of 5-10°C, then transfer to a vacuum drying oven and dry at 35-45°C for 24 h, sieve and powder to obtain component A.
制备组分B:将消泡剂、催化剂、引发剂与剩余陶瓷粉体混合,在5-10℃的温度下,以100-150r/min的速度搅拌1.5-2.5h,随后转移至低温干燥箱中以35-45℃的温度条件干燥24h,过筛后打粉,得到组分B。Preparation of component B: Mix the defoamer, catalyst, initiator and remaining ceramic powder, stir at 100-150 r/min for 1.5-2.5 h at a temperature of 5-10°C, then transfer to a low-temperature drying oven and dry at 35-45°C for 24 h, sieve and powder to obtain component B.
碳化硅陶瓷制备:将上述制备得到的组分A与组分B以质量比为(3.8-4.2):1的比例倒入点胶机或注塑机内,在点胶机或注塑机的推力下,使得组分A与组分B粉体混合,在点胶机或注塑机的出口处设置加水口,加入去离子水后,组分A与组分B之阿金组合在一起形成整体,并进行固化,产品成型得到坯体,将剩余的组分A与组分B回收;成型后的坯体恒温恒湿干燥,干燥制度如表1;干燥技术后,将坯体进行无压烧结,控制烧结温度为2100-2200℃,保温时间为2-5h,得到碳化硅陶瓷产品。Preparation of silicon carbide ceramics: The components A and B prepared above are poured into a dispensing machine or an injection molding machine at a mass ratio of (3.8-4.2):1. Under the thrust of the dispensing machine or the injection molding machine, the powders of components A and B are mixed. A water inlet is set at the outlet of the dispensing machine or the injection molding machine. After adding deionized water, components A and B are combined together to form a whole, and then cured. The product is formed to obtain a green body, and the remaining components A and B are recovered; the green body after forming is dried at a constant temperature and humidity, and the drying system is shown in Table 1; after the drying technology, the green body is pressurelessly sintered, the sintering temperature is controlled to be 2100-2200°C, and the insulation time is 2-5h to obtain a silicon carbide ceramic product.
表1 坯体干燥制度Table 1 Green body drying system
实施例Example
制备碳化硅表面改性超细粉:Preparation of silicon carbide surface modified ultrafine powder:
将1890.8g的碳化硅超细粉与2000ml的去离子水混合,使用氢氧化钠调节pH值至10,以300rpm的转速搅拌30min,随后加入35.91g的二甲基二丙烯基氯化铵-丙烯酰胺共聚物(CAS号:26590-05-6)和73.29g的月桂醇硫酸钠(CAS号:151-21-3),加热至88℃后以400rpm的转速搅拌4h,离心后使用去离子水洗涤沉淀,重复洗涤两次后,将得到的沉淀物在80℃的温度下干燥24h,研磨后得到碳化硅表面改性超细粉。1890.8g of silicon carbide ultrafine powder was mixed with 2000ml of deionized water, and the pH value was adjusted to 10 with sodium hydroxide. The mixture was stirred at 300rpm for 30min, and then 35.91g of dimethyldiallylammonium chloride-acrylamide copolymer (CAS No.: 26590-05-6) and 73.29g of sodium lauryl sulfate (CAS No.: 151-21-3) were added. The mixture was heated to 88°C and stirred at 400rpm for 4h. After centrifugation, the precipitate was washed with deionized water. After repeated washing twice, the precipitate was dried at 80°C for 24h and ground to obtain silicon carbide surface modified ultrafine powder.
制备陶瓷粉体:将1753.11g上述制备的碳化硅表面改性超细粉、36.07g炭黑与10.82g氮化碳粉体混合后,得到陶瓷粉体。Preparation of ceramic powder: 1753.11 g of the above-prepared silicon carbide surface-modified ultrafine powder, 36.07 g of carbon black and 10.82 g of carbon nitride powder were mixed to obtain ceramic powder.
制备碳化硅陶瓷:Preparation of silicon carbide ceramics:
制备组分A:将41g的丙烯酰胺、4g的亚甲基双丙烯酰胺、200g的去离子水、30g的分散剂、7.5g的悬浮剂以及905g的陶瓷粉体混合,在5℃的温度下,以150r/min的速度搅拌1.5h,随后转移至真空干燥箱中以40℃的温度条件干燥24h,过筛后打粉,得到组分A。Preparation of component A: Mix 41 g of acrylamide, 4 g of methylenebisacrylamide, 200 g of deionized water, 30 g of dispersant, 7.5 g of suspending agent and 905 g of ceramic powder, stir at 150 r/min for 1.5 h at 5 °C, then transfer to a vacuum drying oven and dry at 40 °C for 24 h, sieve and powder to obtain component A.
制备组分B:将0.75g的消泡剂、0.075g的催化剂、0.08g的引发剂与312g的陶瓷粉体混合,在5℃的温度下,以150r/min的速度搅拌1.5h,随后转移至真空干燥箱中以35℃的温度条件干燥24h,过筛后打粉,得到组分B。Preparation of component B: Mix 0.75 g of defoamer, 0.075 g of catalyst, 0.08 g of initiator and 312 g of ceramic powder, stir at 150 r/min for 1.5 h at 5 °C, then transfer to a vacuum drying oven and dry at 35 °C for 24 h, sieve and powder to obtain component B.
碳化硅陶瓷制备:称取上述制备得到的1187.5g组分A、312.5g组分B加入至注塑机中,启动注塑机后使得组分A与组分B充分混合,在注塑机出口处设置加水口,加入200g的去离子水,组分A、组分B在去离子水的作用下形成整体并固化,根据制备需求得到坯体,回收剩余的组分A与组分B;将得到的坯体恒温恒湿至干燥,干燥制度参选表1;干燥结束后,进行无压烧结,控制烧结温度为2100℃,保温时间为5h,得到碳化硅陶瓷产品。Preparation of silicon carbide ceramics: Weigh 1187.5g of component A and 312.5g of component B prepared above and add them to an injection molding machine. After starting the injection molding machine, fully mix component A and component B. Set a water inlet at the outlet of the injection molding machine, add 200g of deionized water, and component A and component B form a whole and solidify under the action of deionized water. Obtain a green body according to the preparation requirements, and recover the remaining component A and component B; keep the obtained green body at a constant temperature and humidity until it is dry, and the drying system is shown in Table 1; after drying, perform pressureless sintering, control the sintering temperature to 2100°C, and the insulation time to 5h to obtain a silicon carbide ceramic product.
实施例Example
制备碳化硅表面改性超细粉:Preparation of silicon carbide surface modified ultrafine powder:
将1889.42g的碳化硅超细粉与2000ml的去离子水混合,使用氢氧化钠调节pH值至10,以300rpm的转速搅拌30min,随后加入37.35g的二甲基二丙烯基氯化铵-丙烯酰胺共聚物和73.23g的月桂醇硫酸钠,加热至92℃后以400rpm的转速搅拌4h,离心后使用去离子水洗涤沉淀,重复洗涤两次后,将得到的沉淀物在80℃的温度下干燥24h,研磨后得到碳化硅表面改性超细粉。1889.42 g of silicon carbide ultrafine powder was mixed with 2000 ml of deionized water, and the pH value was adjusted to 10 with sodium hydroxide. The mixture was stirred at 300 rpm for 30 min, and then 37.35 g of dimethyldiacrylammonium chloride-acrylamide copolymer and 73.23 g of sodium lauryl sulfate were added. The mixture was heated to 92°C and stirred at 400 rpm for 4 h. After centrifugation, the precipitate was washed with deionized water. After repeated washing twice, the precipitate was dried at 80°C for 24 h and ground to obtain silicon carbide surface modified ultrafine powder.
制备陶瓷粉体:将1753.29g上述制备的碳化硅表面改性超细粉、35.93g炭黑与10.78g氮化碳粉体混合后,得到陶瓷粉体。Preparation of ceramic powder: 1753.29 g of the silicon carbide surface-modified ultrafine powder prepared above, 35.93 g of carbon black and 10.78 g of carbon nitride powder were mixed to obtain ceramic powder.
制备碳化硅陶瓷:Preparation of silicon carbide ceramics:
制备组分A:将100.7g的丙烯酰胺、6.8g的亚甲基双丙烯酰胺、270g的去离子水、150g的分散剂、11g的悬浮剂以及1181.5g的陶瓷粉体混合,在10℃的温度下,以100r/min的速度搅拌1.5h,随后转移至真空干燥箱中以40℃的温度条件干燥24h,过筛后打粉,得到组分A。Preparation of component A: Mix 100.7 g of acrylamide, 6.8 g of methylenebisacrylamide, 270 g of deionized water, 150 g of dispersant, 11 g of suspending agent and 1181.5 g of ceramic powder, stir at 100 r/min for 1.5 h at 10°C, then transfer to a vacuum drying oven and dry at 40°C for 24 h, sieve and powder to obtain component A.
制备组分B:将6.45g的消泡剂、0.215g的催化剂、0.2g的引发剂与423g的陶瓷粉体混合,在10℃的温度下,以100r/min的速度搅拌1.5h,随后转移至真空干燥箱中以45℃的温度条件干燥24h,过筛后打粉,得到组分B。Preparation of component B: Mix 6.45 g of defoamer, 0.215 g of catalyst, 0.2 g of initiator and 423 g of ceramic powder, stir at 100 r/min for 1.5 h at 10°C, then transfer to a vacuum drying oven and dry at 45°C for 24 h, sieve and powder to obtain component B.
碳化硅陶瓷制备:称取上述制备得到的1720g组分A、430g组分B加入至注塑机中,启动注塑机后使得组分A与组分B充分混合,在注塑机出口处设置加水口,加入200g的去离子水,组分A、组分B在去离子水的作用下形成整体并固化,根据制备需求得到坯体,回收剩余的组分A与组分B;将得到的坯体恒温恒湿至干燥,干燥制度参选表1;干燥结束后,进行无压烧结,控制烧结温度为2100℃,保温时间为5h,得到碳化硅陶瓷产品。Preparation of silicon carbide ceramics: Weigh 1720g of component A and 430g of component B prepared above and add them to an injection molding machine. After starting the injection molding machine, fully mix component A and component B. Set a water inlet at the outlet of the injection molding machine, add 200g of deionized water, and component A and component B form a whole and solidify under the action of deionized water. A green body is obtained according to the preparation requirements, and the remaining component A and component B are recovered; the obtained green body is kept at a constant temperature and humidity until dry, and the drying system is shown in Table 1; after drying, pressureless sintering is carried out, the sintering temperature is controlled to 2100°C, and the insulation time is 5h to obtain a silicon carbide ceramic product.
实施例Example
制备碳化硅表面改性超细粉:Preparation of silicon carbide surface modified ultrafine powder:
将1890.11g的碳化硅超细粉与2000ml的去离子水混合,使用氢氧化钠调节pH值至10,以300rpm的转速搅拌30min,随后加入36.63g的二甲基二丙烯基氯化铵-丙烯酰胺共聚物和73.26g的月桂醇硫酸钠,加热至90℃后以400rpm的转速搅拌4h,离心后使用去离子水洗涤沉淀,重复洗涤两次后,将得到的沉淀物在80℃的温度下干燥24h,研磨后得到碳化硅表面改性超细粉。1890.11 g of silicon carbide ultrafine powder was mixed with 2000 ml of deionized water, and the pH value was adjusted to 10 with sodium hydroxide. The mixture was stirred at 300 rpm for 30 min, and then 36.63 g of dimethyldiacrylammonium chloride-acrylamide copolymer and 73.26 g of sodium lauryl sulfate were added. The mixture was heated to 90°C and stirred at 400 rpm for 4 h. After centrifugation, the precipitate was washed with deionized water. After repeated washing twice, the precipitate was dried at 80°C for 24 h and ground to obtain silicon carbide surface modified ultrafine powder.
制备陶瓷粉体:将1753.2g上述制备的碳化硅表面改性超细粉、36g炭黑与10.8g氮化碳粉体混合后,得到陶瓷粉体。Preparation of ceramic powder: 1753.2 g of the above-prepared silicon carbide surface-modified ultrafine powder, 36 g of carbon black and 10.8 g of carbon nitride powder were mixed to obtain ceramic powder.
制备碳化硅陶瓷:Preparation of silicon carbide ceramics:
制备组分A:将68.5g的丙烯酰胺、5.5g的亚甲基双丙烯酰胺、250g的去离子水、65g的分散剂、9.5g的悬浮剂以及1096.5g的陶瓷粉体混合,在7℃的温度下,以130r/min的速度搅拌1.5h,随后转移至真空干燥箱中以40℃的温度条件干燥24h,过筛后打粉,得到组分A。Preparation of component A: Mix 68.5 g of acrylamide, 5.5 g of methylenebisacrylamide, 250 g of deionized water, 65 g of dispersant, 9.5 g of suspending agent and 1096.5 g of ceramic powder, stir at 130 r/min at 7°C for 1.5 h, then transfer to a vacuum drying oven and dry at 40°C for 24 h, sieve and powder to obtain component A.
制备组分B:将3.7g的消泡剂、0.15g的催化剂、0.15g的引发剂与351g的陶瓷粉体混合,在7℃的温度下,以130r/min的速度搅拌1.5h,随后转移至真空干燥箱中以40℃的温度条件干燥24h,过筛后打粉,得到组分B。Preparation of component B: Mix 3.7 g of defoamer, 0.15 g of catalyst, 0.15 g of initiator and 351 g of ceramic powder, stir at 130 r/min at 7°C for 1.5 h, then transfer to a vacuum drying oven and dry at 40°C for 24 h, sieve and powder to obtain component B.
碳化硅陶瓷制备:称取上述制备得到的1495g组分A、355g组分B加入至注塑机中,启动注塑机后使得组分A与组分B充分混合,在注塑机出口处设置加水口,加入200g的去离子水,组分A、组分B在去离子水的作用下形成整体并固化,根据制备需求得到坯体,回收剩余的组分A与组分B;将得到的坯体恒温恒湿至干燥,干燥制度参选表1;干燥结束后,进行无压烧结,控制烧结温度为2100℃,保温时间为5h,得到碳化硅陶瓷产品。Preparation of silicon carbide ceramics: Weigh 1495g of component A and 355g of component B prepared above and add them to an injection molding machine. After starting the injection molding machine, fully mix component A and component B. Set a water inlet at the outlet of the injection molding machine, add 200g of deionized water, and component A and component B form a whole and solidify under the action of deionized water. A green body is obtained according to the preparation requirements, and the remaining component A and component B are recovered; the obtained green body is kept at a constant temperature and humidity until dry, and the drying system is shown in Table 1; after drying, pressureless sintering is carried out, the sintering temperature is controlled to 2100°C, and the insulation time is 5h to obtain a silicon carbide ceramic product.
实施例Example
实施例4以实施例3为基准,实施例4与实施例3之间的区别在于,实施例4中在制备碳化硅表面改性超细粉时,称取的二甲基二丙烯基氯化铵-丙烯酰胺共聚物为33.03g,称取的月桂醇硫酸钠为73.39g。Example 4 is based on Example 3. The difference between Example 4 and Example 3 is that in Example 4, when preparing the surface-modified silicon carbide ultrafine powder, the dimethyldiacrylammonium chloride-acrylamide copolymer weighed is 33.03 g, and the sodium lauryl sulfate weighed is 73.39 g.
实施例Example
实施例5以实施例3为基准,实施例5与实施例3之间的区别在于,实施例5中在制备碳化硅表面改性超细粉时,称取的二甲基而丙烯氯化铵-丙烯酰胺共聚物为40.22g,称取的月桂醇硫酸钠为73.13g。Example 5 is based on Example 3. The difference between Example 5 and Example 3 is that in Example 5, when preparing the surface-modified silicon carbide ultrafine powder, the amount of dimethyl propylene ammonium chloride-acrylamide copolymer weighed is 40.22 g, and the amount of sodium lauryl sulfate weighed is 73.13 g.
实施例Example
实施例6以实施例3为基准,实施例6与实施例3之间的区别在于,实施例6中在制备碳化硅表面改性超细粉时,称取的二甲基而丙烯氯化铵-丙烯酰胺共聚物为36.9g,称取的月桂醇硫酸钠为59.04g。Example 6 is based on Example 3. The difference between Example 6 and Example 3 is that in Example 6, when preparing the surface-modified ultrafine powder of silicon carbide, 36.9 g of dimethyl propylene ammonium chloride-acrylamide copolymer is weighed, and 59.04 g of sodium lauryl sulfate is weighed.
实施例Example
实施例7以实施例3为基准,实施例7与实施例3之间的区别在于,实施例7中在制备碳化硅表面改性超细粉时,称取的二甲基而丙烯氯化铵-丙烯酰胺共聚物为36.36g,称取的月桂醇硫酸钠为87.27g。Example 7 is based on Example 3. The difference between Example 7 and Example 3 is that in Example 7, when preparing the surface-modified silicon carbide ultrafine powder, 36.36 g of dimethyl propylene ammonium chloride-acrylamide copolymer is weighed, and 87.27 g of sodium lauryl sulfate is weighed.
实施例Example
实施例8以实施例3为基准,实施例8与实施例3的区别在于,实施例8中在制备碳化硅表面改性超细粉时,将月桂醇硫酸钠替换为等量的双琥珀酰亚胺辛二酸酯(CAS号:68528-80-3)。Example 8 is based on Example 3. The difference between Example 8 and Example 3 is that in Example 8, when preparing the surface-modified ultrafine powder of silicon carbide, sodium lauryl sulfate is replaced by an equal amount of disuccinimidyl suberate (CAS No.: 68528-80-3).
实施例Example
实施例9以实施例3为基准,实施例9与实施例3的区别在于,实施例9中在制备碳化硅表面改性超细粉时,将月桂醇硫酸钠替换为等量的十二烷基苯磺酸钠(CAS号:25155-30-0)。Example 9 is based on Example 3. The difference between Example 9 and Example 3 is that in Example 9, when preparing the surface-modified ultrafine powder of silicon carbide, sodium lauryl sulfate is replaced by an equal amount of sodium dodecylbenzene sulfonate (CAS No.: 25155-30-0).
实施例Example
实施例10以实施例3为基准,实施例10与实施例3的区别在于:实施例10中在制备碳化硅表面改性超细粉时,将二甲基而丙烯氯化铵-丙烯酰胺共聚物替换为等量的聚二甲基二烯丙基氯化铵(CAS号:26062-79-3)。Example 10 is based on Example 3. The difference between Example 10 and Example 3 is that in Example 10, when preparing the surface-modified ultrafine powder of silicon carbide, the dimethyl propylene ammonium chloride-acrylamide copolymer is replaced with an equal amount of polydimethyldiallylammonium chloride (CAS No.: 26062-79-3).
实施例Example
实施例11以实施例3为基准,实施例11与实施例3的区别在于:实施例11中在制备碳化硅表面改性超细粉时,反应温度为96℃。Example 11 is based on Example 3. The difference between Example 11 and Example 3 is that in Example 11, when preparing the surface-modified silicon carbide ultrafine powder, the reaction temperature is 96°C.
实施例Example
实施例12以实施例3为基准,实施例12与实施例3的区别在于:实施例12中在制备碳化硅表面改性超细粉时,反应温度为84℃。Example 12 is based on Example 3. The difference between Example 12 and Example 3 is that in Example 12, when preparing the surface-modified silicon carbide ultrafine powder, the reaction temperature is 84°C.
对比例1Comparative Example 1
对比例1以实施例3为基准,对比例1与实施例3的区别在于:对比例1中未分成组分A与组分B,对比例1中直接将全部原料混合后投入至注塑机中。Comparative Example 1 is based on Example 3. The difference between Comparative Example 1 and Example 3 is that: in Comparative Example 1, component A and component B are not separated. In Comparative Example 1, all raw materials are directly mixed and then put into the injection molding machine.
性能检测试验Performance testing
对实施例1-12,对比例1制备得到碳化硅陶瓷进行取样,并进行如下性能测试:For Examples 1-12 and Comparative Example 1, the silicon carbide ceramics prepared were sampled and subjected to the following performance tests:
(1)以《GB/T 25995-2010精细陶瓷密度和显气孔率试验方法》为检测标准对试样密度进行测试,每份试样检测三次,取平均值,并将检测结果填写至表2。(1) The density of the samples was tested according to the test standard GB/T 25995-2010 Test method for density and apparent porosity of fine ceramics. Each sample was tested three times, and the average value was taken. The test results were filled in Table 2.
(2)以《GB/T 6569-2006精细陶瓷弯曲强度试验方法》为检测标准,对试样进行抗弯强度测试,在室温下,每份试样测试三次,取平均值,并将检测结果填写至表2。(2) Using GB/T 6569-2006 Fine Ceramics Bending Strength Test Method as the test standard, the samples were tested for bending strength. Each sample was tested three times at room temperature, and the average value was taken. The test results were filled in Table 2.
表2 实施例1-12与对比例碳化硅陶瓷性能测试结果Table 2 Performance test results of silicon carbide ceramics of Examples 1-12 and Comparative Examples
数据分析Data analysis
由表1可知,实施例1-3所制备得到的碳化硅陶瓷密度均值在3.13g/cm3及以上,侧壁密度与底部密度的差值均在0.02g/cm3及以下,抗压强度在430MPa以上,说明本申请所制备的碳化硅陶瓷均度良好,产品质量得到明显提升。It can be seen from Table 1 that the average density of the silicon carbide ceramics prepared in Examples 1-3 is 3.13 g/cm 3 or above, the difference between the side wall density and the bottom density is 0.02 g/cm 3 or below, and the compressive strength is above 430 MPa, indicating that the silicon carbide ceramics prepared in this application have good uniformity and the product quality is significantly improved.
当月桂醇硫酸钠的添加量过少时,其富集在碳化硅超细粉体表面后,正吸附现象有所下降,对于碳化硅超细粉体的排斥作用下降,故制备得到的浆料的粉体分散性能与悬浮稳定性有所下降,影响后续制备得到的产品质量;由于月桂醇硫酸钠具有一定的发泡性能,当月桂醇硫酸钠的添加量过多时,制备得到的浆料会产生气泡,过多的气泡形成气团,阻碍了浆料的流动性,浆料粘度过大,体系均度下降,影响了平均密度与产品质量,故实施例4与实施例5的各项性能均有所下降。When the addition amount of sodium lauryl sulfate is too small, after it is enriched on the surface of silicon carbide ultrafine powder, the positive adsorption phenomenon decreases, and the repulsion effect on silicon carbide ultrafine powder decreases, so the powder dispersion performance and suspension stability of the prepared slurry decrease, affecting the quality of the subsequent prepared products; since sodium lauryl sulfate has certain foaming properties, when the addition amount of sodium lauryl sulfate is too much, the prepared slurry will produce bubbles, and too many bubbles will form air masses, which hinder the fluidity of the slurry, the viscosity of the slurry is too large, and the uniformity of the system decreases, affecting the average density and product quality, so the performance of Examples 4 and 5 are all reduced.
当二甲基而丙烯氯化铵-丙烯酰胺共聚物的添加量过少时,难以促进碳化硅超细粉体得到更好的清水性与空间位阻,因此碳化硅超细粉的分散性能有所下降,影响了体系稳定性;当二甲基而丙烯氯化铵-丙烯酰胺共聚物的含量过多时,过高的聚合物浓度会加剧高分子链桥接和重叠,阻碍了浆料的流动性,使得浆料粘度过大,体系均度下降,进而影响产品质量,故实施例6与实施例7的各项性能均有所下降。When the addition amount of dimethyl propylene ammonium chloride-acrylamide copolymer is too small, it is difficult to promote the silicon carbide ultrafine powder to obtain better water-clearing property and steric hindrance, so the dispersion performance of the silicon carbide ultrafine powder is reduced, affecting the stability of the system; when the content of dimethyl propylene ammonium chloride-acrylamide copolymer is too much, the excessively high polymer concentration will aggravate the bridging and overlapping of the polymer chains, hinder the fluidity of the slurry, make the slurry viscosity too large, and reduce the uniformity of the system, thereby affecting the product quality. Therefore, the various performances of Example 6 and Example 7 are reduced.
双琥珀酰亚胺辛二酸酯磺酸基团电离完全率低,阻碍了分子链形成空间位阻构象,因此碳化硅超细粉体的分散性能提升效果下降;十二烷基苯磺酸钠的氢键作用较弱,也会影响碳化硅超细粉体的空间位阻构象,进而使得碳化硅超细粉体的分散效果下降,因此实施例8与实施例9体系的稳定性改善效果均有所下降,各项性能有所下降。The complete ionization rate of disuccinimidyl suberate sulfonic acid group is low, which hinders the molecular chain from forming a sterically hindered conformation, and thus the effect of improving the dispersion performance of the silicon carbide ultrafine powder is reduced; the hydrogen bonding effect of sodium dodecylbenzene sulfonate is relatively weak, which will also affect the sterically hindered conformation of the silicon carbide ultrafine powder, thereby reducing the dispersion effect of the silicon carbide ultrafine powder. Therefore, the stability improvement effects of the systems of Example 8 and Example 9 are both reduced, and various performances are reduced.
聚二甲基二烯丙基氯化铵具有过多的正电荷基团,在碱性环境中分子链的分散性能有所下降,故对于碳化硅超细粉体的分散性能改性效果难以提升,因此实施例10体系的稳定性有所下降,使得各项性能均有所下降。Polydimethyldiallylammonium chloride has too many positively charged groups, and the dispersion performance of the molecular chain is reduced in an alkaline environment. Therefore, it is difficult to improve the dispersion performance modification effect of silicon carbide ultrafine powder. Therefore, the stability of the system in Example 10 is reduced, resulting in a decrease in various performances.
制备改性碳化硅超细粉时,当反应温度过低,会使得后续碳化硅超细粉体后续制备得到的浆料粘度升高,影响浆料流动性,使得体系整体的稳定性有所下降;当反应温度过高时,体系中高分子聚合物的性能会有所下降,进而影响对碳化硅超细粉体的改性效果,因此实施例11与实施例12的各项性能均有所下降。When preparing modified silicon carbide ultrafine powder, when the reaction temperature is too low, the viscosity of the slurry obtained from the subsequent preparation of the silicon carbide ultrafine powder will increase, affecting the fluidity of the slurry and reducing the overall stability of the system; when the reaction temperature is too high, the performance of the high molecular weight polymer in the system will decrease, thereby affecting the modification effect of the silicon carbide ultrafine powder. Therefore, the performance of Examples 11 and 12 are all reduced.
对比例1中直接将全部原料混合投入至注塑机中,全部原料混合后再投入注塑机内在制备大尺寸碳化硅陶瓷产品时,全部原料固化时整体发热,对于固化效果难以控制,固化均度下降,因此对比例1所制备的产品质量有所下降。In Comparative Example 1, all the raw materials are directly mixed and put into the injection molding machine. When all the raw materials are mixed and then put into the injection molding machine to prepare large-sized silicon carbide ceramic products, all the raw materials generate heat as a whole during curing, and the curing effect is difficult to control. The curing uniformity decreases, and therefore the quality of the product prepared in Comparative Example 1 decreases.
本具体实施例仅仅是对本申请的解释,其并不是对本申请的限制,通过上述的说明内容,相关工作人员完全可以在不偏离本项申请技术思想的范围内,进行多样的变更以及修改。本项申请的技术性范围并不局限于说明书上的内容,必须要根据权利要求范围来确定其技术性范围。This specific embodiment is only an explanation of the present application, and it is not a limitation of the present application. Through the above description, relevant staff can make various changes and modifications without deviating from the technical idea of the present application. The technical scope of the present application is not limited to the content in the specification, and its technical scope must be determined according to the scope of the claims.
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Application publication date: 20240913 |