CN110204318B - 一种基于粉末床熔融的氧化铝多孔材料的强度增强方法 - Google Patents
一种基于粉末床熔融的氧化铝多孔材料的强度增强方法 Download PDFInfo
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Abstract
一种基于粉末床熔融的氧化铝多孔材料的强度增强方法,先将强度增强材料粉末倒入初始原料中混合;然后将混好的原料放入粉末床熔融3D打印机中,按照设计的多孔结构三维模型打印出初坯;再将初坯放入硅溶胶、镁溶胶、钇溶胶或锆溶胶中浸渍,放入抽真空机中抽真空,使初坯充分浸渍;然后将浸渍后的初坯取出,放在烘箱中干燥;最后按照设定的阶梯升温曲线,先对经过预浸渍且干燥的氧化铝多孔材料的初坯进行脱脂处理,再对初坯进行高温焙烧处理,获得强度满足要求的多孔结构;本发明能够制备出强度满足要求的氧化铝多孔材料。
Description
技术领域
本发明属于快速成型中多孔材料的制备技术领域,具体涉及一种基于粉末床熔融的氧化铝多孔材料的强度增强方法。
背景技术
多孔材料是一种表面或材料内部具有大量孔隙的材料,由于其多孔性,具有比表面积大、吸附量高、质量轻、比强度高、渗透性好等优点,可广范应用在离子交换、吸附、过滤与分离、催化剂、传感器、轻质化设计等领域。
目前已经报道了许多具有微观/宏观结构的不同材料,对于大多数这些多孔材料,它们的性能与它们独特的结构密切相关。然而,国内外多孔材料的制备手段相对传统,主要有挤压成形、注浆成形、发泡工艺、添加造孔剂、溶胶-凝胶法(用于纳米级孔径)等,毫无疑问,这些方法的高成本和复杂性阻碍了这些材料的潜在工业应用。制备专门的3D功能结构需要更简单和更灵活的方法,3D打印技术允许精确地制造具有所需构造和优化性能的3D器件,简单化、个性化制造、生产成本低是此方法的其显着优点。
在粉末床熔融制备氧化铝多孔材料领域中,现有技术都直接使用氧化铝作为基体材料,不关注于多孔材料的强度要求,在中国专利《一种基于粉末床熔融的复杂结构多孔陶瓷的制备方法中》(专利号201610687672.3)中,该专利使用氧化铝或堇青石等陶瓷材料直接进行3D打印。在中国专利《一种激光烧结3D打印快速成型氧化铝粉末的制备》(专利号201510284342.5)中,主要聚焦在氧化铝粉末的制备。但是在3D打印多孔材料的过程中,许多多孔材料与打印出来的试件强度不够。
发明内容
为了克服现有技术的缺点,本发明的目的在于提供了一种基于粉末床熔融的氧化铝多孔材料的强度增强方法,能够制备出强度满足要求的氧化铝多孔材料。
为了达到上述目的,本发明采取的技术方案为:
一种基于粉末床熔融的氧化铝多孔材料的强度增强方法,包括以下步骤:
1)将占总粉体质量分数为3~30wt%的强度增强材料粉末倒入初始原料中混合;初始原料包括占总粉质量分数为45~87wt%的基体材料与占总粉质量分数为10~25wt%的粘结剂材料;
强度增强材料为硅粉和含硅的化合物,含镁的材料,含钇的化合物,含锆的化合物中的一种或多种的组合;
2)将步骤1)混好的原料放入粉末床熔融3D打印机中,按照设计的多孔结构三维模型打印出初坯;
3)将初坯放入浓度为5%~40%的硅溶胶、镁溶胶、钇溶胶或锆溶胶中浸渍,放入抽真空机中抽真空,控制抽真空机压强在18000±2000Pa范围内,对应真空表读数为0.082±0.02MPa,保持30min~60min,使初坯充分浸渍;重复进行浸渍,次数为1~3次;
4)将浸渍后的初坯取出,放在烘箱中,恒温40~80℃,干燥3~12小时;
5)按照设定的阶梯升温曲线,先对经过预浸渍且干燥的氧化铝多孔材料的初坯进行脱脂处理,再对初坯进行高温焙烧处理,获得强度满足要求的多孔结构。
所述的步骤1)中强度增强材料粉末的粒径在30nm~40μm范围内。
所述的步骤1)中含硅的化合物为氧化硅或碳酸硅,含镁的材料为氧化镁或碳酸镁,含钇的化合物为氧化钇,含锆的化合物为氧化锆。
所述的步骤1)中基体材料为氢氧化铝粉末、氧化铝粉末中的一种或多种;粘结剂材料为环氧树脂类粉末、尼龙粉末等一种或多种,环氧树脂类粉末为E12或E06。
所述的步骤1)中初始原料粒径为15-100μm。
所述的步骤1)中的原料混合方法为机械混合或干法球磨混合方法,混粉时间3~12小时。
所述的步骤2)中粉末床熔融3D打印机的熔融成形工艺参数为:光斑直径为40μm~300μm,激光功率为5~100W,扫描速度500mm~5000mm/s,扫描间距为0.05~0.3mm,预热温度为50~150摄氏度,分层层厚为0.1~0.2mm。
所述的步骤5)中脱脂工艺为将经过预浸渍且干燥的氧化铝多孔材料的初坯在1~2小时的时间内升至300~350℃,保温0.5~3小时,再在3~4小时的时间内升至550~800℃,保温1~4小时;高温焙烧处理为:脱脂工艺结束后,从550~800℃升至1200~1700℃,保温2~5小时,随炉冷却至室温。
本发明与现有技术相比,具有以下优点及有益效果:
1.粉末床熔融3D打印制备氧化铝多孔材料有别于传统多孔材料的制备方法,这种工艺本身造成的孔隙将转为制造多孔结构优势,较其他3D打印工艺更有优势。整个制造过程无需支撑,可以实现复杂氧化铝多孔材料的大批量、快速制造,大大缩短了产品开发的周期,有利于实现自由设计到制造的一体化。
2.解决了3D打印氧化铝多孔材料强度过低的问题,尤其是3D打印氢氧化铝制备氧化铝多孔材料强度过低的问题,在配方中引入含硅材料、含镁材料、含钇材料,在后续的高温焙烧工艺中,这些材料与氧化铝反应将会生成强化相:莫来石、镁铝尖晶石、钇铝石榴石,利于提高氧化铝多孔材料的强度。在配方中引入含锆材料,在后续的高温焙烧工艺中,会与氧化铝形成氧化锆增韧氧化铝陶瓷,有利于提高多孔氧化铝陶瓷的韧性与强度,其韧化效果主要来源于以下机理:①使氧化铝晶粒基体细化;②氧化锆发生相变韧化;③显微裂纹韧化;④裂纹转向与分叉。
3.本发明将预浸渍工艺引入,将初坯充分浸渍后进行再烧结,充分利用粉末床熔融3D打印这种工艺本身造成的孔隙,使硅溶胶、镁溶胶、钇溶胶中的氧化硅、氧化镁、氧化钇等纳米颗粒充分浸渍到初坯的孔隙中,这些材料与氧化铝反应将会生成强化相:莫来石、镁铝尖晶石、钇铝石榴石,利于提高氧化铝多孔材料的强度。使用锆溶胶中的氧化锆纳米颗粒充分浸渍到初坯的孔隙中,在后续的高温焙烧工艺中,会与氧化铝形成氧化锆增韧氧化铝陶瓷,有利于提高多孔氧化铝陶瓷的韧性与强度。采用预浸渍工艺是因为:一、初坯脱脂后没有强度无法浸渍;二、不在高温焙烧后浸渍,防止高温焙烧后再浸渍再高温焙烧过度影响多孔材料的孔隙结构。
具体实施方式
下面结合实施例对本发明方法作详细描述。
实施例1,一种基于粉末床熔融的氧化铝多孔材料的强度增强方法,包括以下步骤:
1)将400g中位径为5μm的二氧化硅粉末放入1300g中位径为25μm氢氧化铝粉末与300g中位径为15μm环氧树脂粉末中,采用机械混合的方式混合3小时;
2)将步骤1)混好的原料放入粉末床熔融3D打印机中,按照设计的多孔结构三维模型打印出初坯;
采用工艺参数为:预热55℃,层厚0.15mm,激光光斑40μm,激光功率25W,扫描速度2000mm/s,扫描间距20μm;
3)将初坯放入浓度为40%的硅溶胶中浸渍,放入抽真空机中抽真空,控制抽真空机压强在18000Pa,对应真空表读数为0.082MPa,保持30min,使初坯充分浸渍;
4)将浸渍后的初坯取出,放在烘箱中,恒温80℃,干燥3小时;如不进行干燥,则在后续脱脂工艺和高温焙烧工艺中容易引起初坯开裂;
5)按照设定的阶梯升温曲线,先对经过预浸渍且干燥的氧化铝多孔材料的初坯进行脱脂处理,再对初坯进行高温焙烧处理,获得强度满足要求的多孔结构;
脱脂工艺为将经过预浸渍且干燥的氧化铝多孔材料的初坯在2小时升至300℃,保温1小时,再用3小时的时间内升至800℃,保温2小时;高温焙烧处理为:脱脂工艺结束后,从800℃升至1600℃,保温3小时,随炉冷却至室温。
本实施例所得多孔结构在室温23℃下,以1mm/min的速度均匀加载,使用多功能力学实验机进行测试,测得压缩强度为19.824MPa,压碎强度为516.50886N/cm。
实施例2,一种基于粉末床熔融的氧化铝多孔材料的强度增强方法,包括以下步骤:
1)将100g中位径为5μm的氧化锆粉末和100g中位径为5μm的氧化钇粉末放入1600g中位径为25μm氢氧化铝粉末与200g中位径为15μm环氧树脂粉末中,采用干法球磨混合的方式混合5小时;
2)将步骤1)混好的原料放入粉末床熔融3D打印机中,按照设计的多孔结构三维模型打印出初坯;
采用工艺参数为:预热60℃,层厚0.15mm,激光光斑40μm,激光功率20W,扫描速度3000mm/s,扫描间距20μm;
3)将初坯放入浓度为5%的硅溶胶中浸渍,放入抽真空机中抽真空,控制抽真空机压强在18000Pa,对应真空表读数为0.082MPa,保持40min,使初坯充分浸渍;
4)将浸渍后的初坯取出,放在烘箱中,恒温40℃,干燥12小时;如不进行干燥,则在后续脱脂工艺和高温焙烧工艺中容易引起初坯开裂;
5)按照设定的阶梯升温曲线,先对经过预浸渍且干燥的氧化铝多孔材料的初坯进行脱脂处理,再对初坯进行高温焙烧处理,获得强度满足要求的多孔结构;
脱脂工艺为将经过预浸渍且干燥的氧化铝多孔材料的初坯在1小时升至300℃,保温1小时,再用3小时的时间内升至800℃,保温1小时;高温焙烧处理为:脱脂工艺结束后,从800℃升至1400℃,保温2小时,随炉冷却至室温。
本实施例所得多孔结构在室温23℃下,以1mm/min的速度均匀加载,使用多功能力学实验机进行测试,测得压缩强度为25.766MPa,压碎强度为774.76329N/cm。
实施例3,一种基于粉末床熔融的氧化铝多孔材料的强度增强方法,包括以下步骤:
1)将60g中位径为5μm的氧化镁粉末放入1340g中位径为70μm氧化铝粉末与600g中位径为15μm环氧树脂粉末中,采用干法球磨混合的方式混合12小时;
2)将步骤1)混好的原料放入粉末床熔融3D打印机中,按照设计的多孔结构三维模型打印出初坯;
采用工艺参数为:预热50℃,层厚0.15mm,激光光斑40μm,激光功率20W,扫描速度3000mm/s,扫描间距20μm;
3)将初坯放入浓度为10%的硅溶胶中浸渍,放入抽真空机中抽真空,控制抽真空机压强在18000Pa,对应真空表读数为0.082MPa,保持30min,使初坯充分浸渍;
4)将浸渍后的初坯取出,放在烘箱中,恒温50℃,干燥5小时;如不进行干燥,则在后续脱脂工艺和高温焙烧工艺中容易引起初坯开裂;
5)按照设定的阶梯升温曲线,先对经过预浸渍且干燥的氧化铝多孔材料的初坯进行脱脂处理,再对初坯进行高温焙烧处理,获得强度满足要求的多孔结构;
脱脂工艺为将经过预浸渍且干燥的氧化铝多孔材料的初坯在1.5小时升至300℃,保温1小时,再用3小时的时间内升至800℃,保温1小时;高温焙烧处理为:脱脂工艺结束后,从800℃升至1700℃,保温3小时,随炉冷却至室温。
本实施例所得多孔结构在室温23℃下,以1mm/min的速度均匀加载,使用多功能力学实验机进行测试,测得压缩强度为12.523MPa,压碎强度为326.283N/cm。
实施例4,一种基于粉末床熔融的氧化铝多孔材料的强度增强方法,包括以下步骤:
1)将200g中位径为40μm的氧化硅粉末放入750g中位径为25μm氢氧化铝粉末和750g中位径为70μm氢化铝粉末和300g中位径为50μm尼龙粉末中,采用干法球磨混合的方式混合12小时;
2)将步骤1)混好的原料放入粉末床熔融3D打印机中,按照设计的多孔结构三维模型打印出初坯;
采用工艺参数为:预热150℃,层厚0.12mm,激光光斑40μm,激光功率60W,扫描速度3000mm/s,扫描间距20μm;
3)将初坯放入浓度为5%的锆溶胶中浸渍,放入抽真空机中抽真空,控制抽真空机压强在18000Pa,对应真空表读数为0.082MPa,保持30min,使初坯充分浸渍;再将初坯放入浓度为5%的钇溶胶中浸渍,放入抽真空机中抽真空,控制抽真空机压强在18000Pa,对应真空表读数为0.082MPa,保持30min,使初坯充分浸渍;
4)将浸渍后的初坯取出,放在烘箱中,恒温60℃,干燥4小时;如不进行干燥,则在后续脱脂工艺和高温焙烧工艺中容易引起初坯开裂;
5)按照设定的阶梯升温曲线,先对经过预浸渍且干燥的氧化铝多孔材料的初坯进行脱脂处理,再对初坯进行高温焙烧处理,获得强度满足要求的多孔结构;
脱脂工艺为将经过预浸渍且干燥的氧化铝多孔材料的初坯在1.5小时升至350℃,保温1小时,再用3小时的时间内升至750℃,保温1.5小时。高温焙烧处理为:脱脂工艺结束后,从800℃升至1200℃,保温5小时,随炉冷却至室温。
本实施例所得多孔结构在室温23℃下,以1mm/min的速度均匀加载,使用多功能力学实验机进行测试,测得压缩强度为2.776MPa,压碎强度为54.28994N/cm。
以上所述,仅为本发明较佳的实施例,但本发明的保护范围不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (4)
1.一种基于粉末床熔融的氧化铝多孔材料的强度增强方法,其特征在于,包括以下步骤:
1)将占总粉体质量分数为3~30wt%的强度增强材料粉末倒入初始原料中混合;初始原料包括占总粉质量分数为45~87wt%的基体材料与占总粉质量分数为10~25wt%的粘结剂材料;
强度增强材料为硅粉或含硅的化合物,含镁的材料,含钇的化合物,含锆的化合物中的一种或多种的组合;
2)将步骤1)混好的原料放入粉末床熔融3D打印机中,按照设计的多孔结构三维模型打印出初坯;
3)将初坯放入浓度为5%~40%的硅溶胶、镁溶胶、钇溶胶或锆溶胶中浸渍,放入抽真空机中抽真空,控制抽真空机压强在18000±2000Pa范围内,对应真空表读数为0.082±0.02MPa,保持30min~60min,使初坯充分浸渍;重复进行浸渍,次数为1~3次;
4)将浸渍后的初坯取出,放在烘箱中,恒温40~80℃,干燥3~12小时;
5)按照设定的阶梯升温曲线,先对经过预浸渍且干燥的氧化铝多孔材料的初坯进行脱脂处理,再对初坯进行高温焙烧处理,获得强度满足要求的多孔结构;
所述的步骤1)中基体材料为氢氧化铝粉末;粘结剂材料为环氧树脂类粉末、尼龙粉末的一种或多种,环氧树脂类粉末为E12或E06;
所述的步骤1)中初始原料粒径为15-100μm;
所述的步骤2)中粉末床熔融3D打印机的熔融成形工艺参数为:光斑直径为40μm~300μm,激光功率为5~100W,扫描速度500mm~5000mm/s,扫描间距为0.05~0.3mm,预热温度为50~150摄氏度,分层层厚为0.1~0.2mm;
所述的步骤1)中含硅的化合物为氧化硅或碳酸硅,含镁的材料为氧化镁或碳酸镁,含钇的化合物为氧化钇,含锆的化合物为氧化锆。
2.根据权利要求1所述的一种基于粉末床熔融的氧化铝多孔材料的强度增强方法,其特征在于:所述的步骤1)中强度增强材料粉末的粒径在30nm~40μm范围内。
3.根据权利要求1所述的一种基于粉末床熔融的氧化铝多孔材料的强度增强方法,其特征在于:所述的步骤1)中的原料混合方法为机械混合或干法球磨混合方法,混粉时间3~12小时。
4.根据权利要求1所述的一种基于粉末床熔融的氧化铝多孔材料的强度增强方法,其特征在于:所述的步骤5)中脱脂工艺为将经过预浸渍且干燥的氧化铝多孔材料的初坯在1~2小时的时间内升至300~350℃,保温0.5~3小时,再在3~4小时的时间内升至550~800℃,保温1~4小时;高温焙烧处理为:脱脂工艺结束后,从550~800℃升至1200~1700℃,保温2~5小时,随炉冷却至室温。
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