CN109081685B - 一种氧化铝陶瓷及其制备方法 - Google Patents
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- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 5
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- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 4
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Abstract
本发明公开了一种氧化铝陶瓷的制备方法及制得的产品,其特征是,采用凝胶注模工艺制备了高强度且结构均匀的氧化铝陶瓷。其中,注凝体系的单体分别采用了低毒的N‑羟甲基丙烯酰胺和α‑甲基丙烯酸。为提高氧化铝粉体的高温烧结性能,添加了高温烧结助剂。干燥后的氧化铝陶瓷生坯的抗压强度为15~20Mpa,密度为1.5~2.0g/cm3。1500℃烧结后的氧化铝陶瓷的抗压强度为40~60MPa,密度为3.0~3.8g/cm3。采用凝胶注模法制备的氧化铝陶瓷密度高、强度大,并可达到近净成型的目的。
Description
技术领域
本发明属于无机非金属陶瓷技术领域,具体涉及一种氧化铝陶瓷的制备方法及制得的产品。
背景技术
凝胶注模成型技术自20世纪90年代初由美国橡树岭国家实验室提出后, 以坯体组成均匀、强度高、应用范围广泛以及成型的部件可靠、性能好等传统成型方法不可比拟的优势受到各国陶瓷研究工作者的重视。目前, 许多发达国家如美国、日本等已经把该项技术列为国家发展计划。它将高分子聚合理论引入到传统的注浆成型工艺中, 为陶瓷成型提供了新的思路。经过十几年的不断发展, 又提出了多糖大分子、金属鳌合反应等新的凝胶体系。同时在原有的理论基础上, 又发展了水基流延成型、与激光选区烧结成型技术连用(SLS)制备陶瓷部件等新的成型技术。在其应用领域, 由单一组分陶瓷扩大到多组分陶瓷、多孔陶瓷、梯度陶瓷再到复杂陶瓷异型品的制备。虽然它的发展历史较短, 却已得到广泛的应用, 逐渐成为新型陶瓷成型技术的代表。
丙烯酰胺作为凝胶注模单体最先提出,且研究的最为成熟。但丙烯酰胺单体具有神经毒性,易对人体产生损害。因此采用低毒或无毒的有机单体是其发展趋势。已公开的专利号CN 103072182A提供了一种基于结冷胶凝胶的陶瓷凝胶注模方法,虽然使用的单体新颖,但其引发凝胶的过程复杂。李鑫等人在其论文“N-羟甲基丙烯酰胺体系凝胶注模成型氧化铝陶瓷”中虽然采用了低毒性的N-羟甲基丙烯酰胺作为有机单体,但其氧化铝陶瓷的强度仅有32MPa。氧化铝粉体高温下很难烧结致密化,因此需加入适量的烧结助剂促进其烧结。此外,一些研究者通过加入高岭土等物质作为烧结助剂,但实验发现,添加这些物质,干燥过程中易开裂,陶瓷的成型性不好。
发明内容
发明目的:为了克服现有技术中存在的不足,本发明提供一种具备高抗压强度、密度高、硬度大的氧化铝陶瓷及其制备方法。
技术方案:为解决上述技术问题,本发明的一种氧化铝陶瓷,其原料由氧化铝粉体、,其质量比为:(50~60):(0.8~1):(0.8~1): (0.04~0.06) :(0.8~1): (0.45~0.5):( 1~20): (0~60)。
优选的,所选有机单体为N-羟甲基丙烯酰胺或α-甲基丙烯酸。
所述烧结助剂为硅溶胶,铝溶胶,硝酸铝和硝酸镁混合溶液,纳米气相SiO2粉体,金红石型钛白粉中的一种或多种的混合物;其固含量为氧化铝粉体质量的1~2wt%。
优选地,所述催化剂为TEMED。
优选地,所述引发剂为APS。
优选地,所述分散剂为六偏磷酸钠或柠檬酸铵。
优选地,所述交联剂为N,N-亚甲基双丙烯酰胺(MBAM)。上述的氧化铝陶瓷的制备方法,其制备步骤包括如下:
(1)制备氧化铝浓悬浮体:a,在预先配制好的N-羟甲基丙烯酰胺或α-甲基丙烯酸与MBAM 的混合溶液中, 加入适量的分散剂, 然后将Al2O3粉体分散于预混液中;b,在上述溶液中加入一定量的高温烧结助剂溶液,电动搅拌均匀并超声10~20min,得到氧化铝浓悬浮体浆料。
(2)凝胶注模:将上述浆料加入催化剂TEMED 和引发剂APS , 快速搅拌10~20s后注入模具,常温下浆料固化得到坯体。
(3)干燥、热处理:将模具放入恒温干燥箱中60℃干燥5~10h后,脱模,并继续将坯体干燥10~12h,得到生坯。最后将生坯置于马弗炉中以3℃/min升温至1500℃并保温2h,得到致密的氧化铝陶瓷。
有益效果:本发明方法制备的氧化铝陶瓷相比于现有的凝胶注模制备的氧化铝陶瓷,具有以下优点:
(1)本发明制备的氧化铝陶瓷的抗压强度相对于现有技术而言提高50%以上,不会产生开裂等技术问题;
(2)首先使用了前驱体溶液作为烧结助剂并与气相SiO2、钛白粉混合使用,且总添加量仅为氧化铝粉体的1~2%,前驱体溶液可与氧化铝粉体达到纳米级分散,得到的氧化铝陶瓷抗压强度高、密度大,成型性好,接近其理论密度。
附图说明
图1是所制备的氧化铝陶瓷实物图。
具体实施方式
下面结合附图对本发明作更进一步的说明。
实施例一:
事先已制备好的酸性硅溶胶(pH值为3~4,SiO2≥10wt.%),聚合氯化铝溶胶(Al2O3≥17wt.%),将5.62g Al(NO3)3·9H2O和1.92g Mg(NO3)2·6H2O溶于20g水中,得到硝酸镁铝溶液,气相SiO2纳米粉体(粒径在7~40nm,团聚颗粒粒径为200~400nm)和金红石型钛白粉,平均粒径1µm。
称取1g N-羟甲基丙烯酰胺、1g N,N-亚甲基双丙烯酰胺(MBAM)和0.25g六偏磷酸钠溶于25g水中得到预混液, 然后将50g平均粒径为1µm 的Al2O3粉体分散于预混液中;在上述溶液中加入17g的酸性硅溶胶和作为高温烧结助剂,电动搅拌均匀并超声10min;得到氧化铝悬浮体浆料。
将上述浆料中滴加0.04g的TEMED 和由1g APS和5g水配成的溶液 , 快速搅拌10s后注入模具,常温下浆料固化得到坯体。将模具放入恒温干燥箱中60℃干燥5h后,脱模,并继续将坯体干燥10h,得到生坯,表面无裂纹。最后将生坯置于马弗炉中以3℃/min升温至1500℃并保温2h,得到致密氧化铝陶瓷,。
所得到的氧化铝陶瓷生坯的抗压强度约为18MPa,密度为1.85g/cm3。致密氧化铝陶瓷的抗压强度约为50MPa,密度为3.25g/cm3,重烧线变化率,1500℃×2h≤0.3%。所得到的泡沫陶瓷可在1800℃以下长期使用,并可机械加工成相应的产品,如图1所示。
实施例二:
称取1g N-羟甲基丙烯酰胺、1g N,N-亚甲基双丙烯酰胺(MBAM)和0.3g柠檬酸铵溶于25g水中得到预混液, 然后将60g平均粒径为1µm 的Al2O3粉体分散于预混液中;在上述溶液中加入7g的聚合氯化铝溶胶作为高温烧结助剂,电动搅拌均匀并超声20min;得到氧化铝悬浮体浆料。
将上述浆料中滴加0.04g的TEMED 和由1g APS和5g水配成的溶液 , 快速搅拌20s后注入模具,常温下浆料固化得到坯体。将模具放入恒温干燥箱中60℃干燥7h后,脱模,并继续将坯体干燥10h,得到生坯。最后将生坯置于马弗炉中以3℃/min升温至1500℃并保温2h,得到致密氧化铝陶瓷。
所得到的氧化铝陶瓷生坯的抗压强度为15.6MPa,密度为1.6g/cm3。致密氧化铝陶瓷的抗压强度为42MPa,密度为3.0g/cm3,重烧线变化1500℃×2h≤0.3%。
实施例三:
称取5g α-甲基丙烯酸、1g N,N-亚甲基双丙烯酰胺(MBAM)和0.3g六偏磷酸钠溶于25g水中得到预混液, 然后将60g平均粒径为1µm 的Al2O3粉体分散于预混液中;在上述溶液中加入7g的硝酸镁铝溶液作为高温烧结助剂,电动搅拌均匀并超声15min;得到氧化铝悬浮体浆料。
将上述浆料中滴加0.04g的TEMED 和由1g APS和5g水配成的溶液 , 快速搅拌10s后注入模具,常温下浆料固化得到坯体。将模具放入恒温干燥箱中60℃干燥10h后,脱模,并继续将坯体干燥12h,得到生坯。最后将生坯置于马弗炉中以3℃/min升温至1500℃并保温2h,得到致密氧化铝陶瓷。
所得到的氧化铝陶瓷生坯的抗压强度为16.8MPa,密度为1.82g/cm3。致密氧化铝陶瓷的抗压强度为45MPa,密度为3.07g/cm3,重烧线变化1500℃×2h≤0.3%。
实施例四:
称取5g α-甲基丙烯酸、1g N,N-亚甲基双丙烯酰胺(MBAM)和0.25g六偏磷酸钠溶于25g水中得到预混液, 然后将50g平均粒径为1µm 的Al2O3粉体和5g的酸性硅溶胶、0.5g钛白粉分散于预混液中,混合搅拌均匀并超声20min,得到氧化铝悬浮体浆料。
将上述浆料中滴加0.04g的TEMED 和由1g APS和5g水配成的溶液 , 快速搅拌10s后注入模具,常温下浆料固化得到坯体。将模具放入恒温干燥箱中60℃干燥5h后,脱模,并继续将坯体干燥10h,得到生坯。最后将生坯置于马弗炉中以3℃/min升温至1500℃并保温2h,得到致密氧化铝陶瓷。
所得到的氧化铝陶瓷生坯的抗压强度为19MPa,密度为1.83g/cm3。致密氧化铝陶瓷的抗压强度为54MPa,密度为3.72g/cm3,重烧线变化1500℃×2h≤0.3%。
实施例五:
称取1g N-羟甲基丙烯酰胺、1g N,N-亚甲基双丙烯酰胺(MBAM)和0.3g柠檬酸铵溶于25g水中得到预混液, 然后将60g的Al2O3粉体和3g的硝酸镁铝溶液、0.3g纳米气相SiO2粉体分散于预混液中,混合搅拌均匀并超声20min;得到氧化铝悬浮体浆料。
将上述浆料中滴加0.04g的TEMED 和由1g APS和10g水配成的溶液 , 快速搅拌10s后注入模具,常温下浆料固化得到坯体。将模具放入恒温干燥箱中60℃干燥10h后,脱模,并继续将坯体干燥12h,得到生坯。最后将生坯置于马弗炉中以3℃/min升温至1500℃并保温2h,得到致密氧化铝陶瓷。
所得到的氧化铝陶瓷生坯的抗压强度为20MPa,密度为1.77g/cm3。致密氧化铝陶瓷的抗压强度为60MPa,密度为3.75g/cm3,重烧线变化1500℃×2h≤0.3%。
以上所述仅是本发明的优选实施方式,应当指出:对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (9)
1.一种氧化铝陶瓷,其特征在于:制备原料包括以下组分:氧化铝粉体、有机单体、交联剂、催化剂、引发剂、分散剂、烧结助剂和水,其质量比例范围依次为:(50~60):(0.8~1):(0.8~1): (0.04~0.06) :(0.8~1): (0.45~0.5):(1~20): (0~ 60);所述烧结助剂为硅溶胶或铝溶胶或硝酸铝和硝酸镁混合溶液与纳米气相SiO2粉体或金红石型钛白粉的混合物;且硅溶胶或铝溶胶或硝酸铝和硝酸镁混合溶液与纳米气相SiO2粉体或金红石型钛白粉的质量比为10:1,烧结助剂总添加量为氧化铝粉体质量的1~2wt%,所述硅溶胶的pH值为3~4,SiO2≥10wt%。
2.根据权利要求1所述的氧化铝陶瓷,其特征在于:所述有机单体为N-羟甲基丙烯酰胺或α-甲基丙烯酸。
3.根据权利要求1所述的氧化铝陶瓷,其特征在于:所述交联剂为N,N-亚甲基双丙烯酰胺。
4.根据权利要求1所述的氧化铝陶瓷,其特征在于:所述引发剂为过硫酸铵。
5.根据权利要求1所述的氧化铝陶瓷,其特征在于:所述催化剂为四甲基乙二胺。
6.根据权利要求1所述的氧化铝陶瓷,其特征在于:所述分散剂为六偏磷酸钠或柠檬酸铵。
7.一种基于权利要求1所述的氧化铝陶瓷的制备方法,其特征在于制备步骤如下:
(1)制备氧化铝浓悬浮体:a,在已配置好的N-羟甲基丙烯酰胺或α-甲基丙烯酸与N,N-亚甲基双丙烯酰胺的预混液中,加入适量的分散剂,然后将Al2O3粉体分散于预混液中;b,在上述溶液中加入一定量的高温烧结助剂,电动搅拌均匀并超声振动,得到氧化铝浓悬浮体浆料;
(2)凝胶注模:在上述浆料中加入催化剂四甲基乙二胺和引发剂过硫酸铵溶液,快速搅拌10~20s后注入模具,常温下浆料固化得到坯体;
(3)干燥、高温烧结:将模具放入恒温干燥箱中60℃干燥5~10h后,脱模,并继续将坯体干燥10~12h,得到生坯,最后将生坯置于马弗炉中以3℃/min升温至1500℃并保温2h,得到氧化铝陶瓷。
8.一种基于权利要求7所述的氧化铝陶瓷的制备方法,其特征在于:在已配置好的单体N-羟甲基丙烯酰胺或α-甲基丙烯酸与交联剂N,N-亚甲基双丙烯酰胺的预混液中,单体、交联剂与水的质量比为:(1~5):1:(20~30)。
9.根据权利要求8所述的氧化铝陶瓷的制备方法,其特征在于:氧化铝陶瓷生坯的抗压强度为15~20MPa,密度为1.5~2.0g/cm3,1500℃烧结后的氧化铝陶瓷的抗压强度为40~60MPa,密度为3.0~3.8g/cm3。
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