CN116573951A - 一种基于光固化成型的陶瓷-树脂复合材料及其制备方法 - Google Patents
一种基于光固化成型的陶瓷-树脂复合材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种基于光固化成型的陶瓷‑树脂复合材料及其制备方法,涉及复合材料技术领域。方法包括:将陶瓷粉体、第一光固化树脂和光引发剂混合制成陶瓷浆料,使用光固化成型打印机制备根据预设的结构图纸光固化成型具有连通孔结构的陶瓷坯体,依次对陶瓷坯体执行脱脂处理和烧结处理,获得陶瓷基体;将陶瓷基体浸渍在充满树脂混合液的容器中,使得树脂混合液浸渗到陶瓷基体的孔隙中,并将树脂混合液固化为树脂材料;清理陶瓷基体周围固化的树脂材料。该方法突破了传统方法制备陶瓷‑树脂复合材料对陶瓷基体的孔隙结构设计自由度的限制,实现树脂材料和陶瓷材料相互连通,有利于发挥陶瓷‑树脂复合材料的强韧化效果,提高陶瓷器件的可靠性。
Description
技术领域
本发明涉及复合材料技术领域,尤其涉及一种基于光固化成型的陶瓷-树脂复合材料及其制备方法。
背景技术
陶瓷-树脂复合材料因其高强度、高韧性、抗磨损等优良性能,在航空航天、汽车制造、医疗器械等领域得到广泛应用。在这种复合材料中,陶瓷可以提供高硬度以及高强度,而树脂材料则可以保持陶瓷结构完整性,能够提供较高的能量吸收,提高断裂韧性,防止灾难性破坏。
其中,陶瓷-树脂复合材料的制备方法对其性能表现具有重要影响。传统的制备方法主要包括冷冻铸造法、注射法、浸渍法以及压电沉积法等,这些方法的制备难度大、成本高、制品尺寸和形状限制较大,难以实现同种材料层相互连通以及孔结构的自由设计。
发明内容
本发明实施例提供了一种基于光固化成型的陶瓷-树脂复合材料及其制备方法,旨在解决目前的陶瓷-树脂复合材料的制备方法对制品尺寸和形状限制较大,难以实现同种材料层相互连通以及孔结构的自由设计的问题。
第一方面,本发明实施例提供了一种基于光固化成型的陶瓷-树脂复合材料的制备方法,包括:
步骤1,将陶瓷粉体、第一光固化树脂和光引发剂混合制成陶瓷浆料,基于所述陶瓷浆料,使用光固化成型打印机制备根据预设的结构图纸光固化成型具有连通孔结构的陶瓷坯体,依次对陶瓷坯体执行脱脂处理和烧结处理,获得陶瓷基体;
步骤2,将所述陶瓷基体浸渍在充满树脂混合液的容器中,使得所述树脂混合液浸渗到所述陶瓷基体的孔隙中,并将所述树脂混合液固化为树脂材料;
步骤3,清理所述陶瓷基体周围固化的树脂材料,获得陶瓷-树脂复合材料。
其中,结构图纸可通过建模软件设计。步骤3具体是指清理陶瓷基体外表面固化的树脂材料。
其进一步的技术方案为,所述步骤1中,采用球磨方式将陶瓷粉体、第一光固化树脂和光引发剂混合制成陶瓷浆料,其中,球磨时间为4-6h,球磨转速为200-350r/min,陶瓷浆料的固含量为40-60vol%。
其进一步的技术方案为,所述步骤1中,光固化成型的曝光时间为2-4s,紫外光光强为7-15mW/cm2。
其进一步的技术方案为,所述步骤1中,脱脂处理的工艺为空气脱脂,包括:以升温速率为0.5℃/min升温,每升温100℃保温1h,直至升至最高温度550-600℃,在最高温度保温6h;然后以0.5℃/min降温至200℃,最后随炉冷却;
所述步骤1中,烧结处理的工艺为无压烧结,包括:以5℃/min升温至1400-1650℃,保温2h;然后以5℃/min降温至800℃,最后随炉冷却。
其进一步的技术方案为,所述树脂混合液包括热固化树脂、塑化剂以及热引发剂,或者,所述树脂混合液包括第二光固化树脂、塑化剂以及光引发剂;所述热引发剂为胺类固化剂,例如乙二胺、三乙烯四胺和乙烯基三胺等;所述光引发剂2,4,6-三甲基苯甲酰基-二苯基氧化膦、2,4,6-三甲基苯甲酰基以及二异丙基二氨基苯甲酰化物中的至少一种,所述塑化剂为邻苯二甲酸二丁酯、聚乙二醇以及2-羟基乙基丙烯酸三甲酯中的至少一种;所述热固化树脂为双酚A型环氧树脂、环氧树脂以及酚醛树脂中的至少一种;所述第二光固化树脂为季戊四醇四丙烯酸酯、三羟甲基丙烷三丙烯酸酯以及1,6-己二醇二丙烯酸酯中的至少一种。
其进一步的技术方案为,以质量份计,所述树脂混合液包括热固化树脂60-80份,塑化剂10-30份,热引发剂10-20份,所述树脂混合液固化过程的工艺参数包括固化温度为100-350℃,固化时间为0.5-4h;
或者,以质量份计,所述树脂混合液包括第二光固化树脂60-80份,塑化剂20-40份,光引发剂1-5份,所述树脂混合液固化过程的工艺参数包括照射时间为0.5-4h,紫外光光强为15-20mW/cm2。
需要说明的是,本发明中,第一光固化树脂可以是其他常用的光固化树脂,也可以与第二光固化树脂相同。例如乙氧化季戍四醇四丙烯酸酯,环氧丙烯酸酯、丙烯酸正丁酯、丙烯酸异辛酯、甲基丙烯酸羟乙酯、甲基丙烯酸羟丙酯、醋酸乙烯酯、乙烯基吡咯烷酮、己二醇二丙烯酸酯、季戊四醇四丙烯酸酯、聚氨酯丙烯酸酯、新戊二醇二丙烯酸酯、二季戊四醇六丙烯酸酯、三羟甲基丙烷三丙烯酸酯以及1,6-己二醇二丙烯酸酯中的至少一种。
其进一步的技术方案为,所述步骤2中,所述树脂混合液浸渍过程的工艺参数包括真空度为0.01-0.1MPa,浸渗时间为10-48h。
其进一步的技术方案为,所述陶瓷基体内部包括相互连通的孔,所述孔的孔径为微米级(10-100μm)或者毫米级(1-50mm),所述孔的截面形状为圆形、方形、椭圆形和不规则形状中的至少一种。
第二方面,本发明实施例还提供了一种陶瓷-树脂复合材料,由第一方面所述的方法制备。
其进一步的技术方案为,所述陶瓷-树脂复合材料包括陶瓷基体以及树脂,所述陶瓷基体包括氧化锆陶瓷或者氧化铝陶瓷中的至少一种;以体积分数计,陶瓷基体的含量为50-80%。
所述陶瓷-树脂复合材料的抗弯强度为500-700MPa,断裂韧性为6-20MPa·m1/2。
与现有的技术相比,本发明使用光固化技术制备具有微米或毫米级别孔隙和连通孔隙结构的陶瓷基体,再通过控制浸渗树脂的方式来实现连通孔隙结构的填充。最终获得了同层材料相互连接,内部为微米或者毫米尺度的陶瓷-树脂复合材料。该方法突破了传统方法制备陶瓷-树脂复合材料对陶瓷基体的孔隙结构设计自由度的限制,实现树脂材料和陶瓷材料相互连通,有利于发挥陶瓷-树脂复合材料的强韧化效果,提高陶瓷器件的可靠性。
附图说明
为了更清楚地说明本发明实施例技术方案,下面将对实施例描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。
图1为本发明实施例提供的陶瓷坯体的设计图;
图2为本发明实施例提供的陶瓷坯体的另一设计图。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
应当理解,当在本说明书和所附权利要求书中使用时,术语“包括”和“包含”指示所描述特征、整体、步骤、操作、元素和/或组件的存在,但并不排除一个或多个其它特征、整体、步骤、操作、元素、组件和/或其集合的存在或添加。
还应当理解,在此本发明说明书中所使用的术语仅仅是出于描述特定实施例的目的而并不意在限制本发明。如在本发明说明书和所附权利要求书中所使用的那样,除非上下文清楚地指明其它情况,否则单数形式的“一”、“一个”及“该”意在包括复数形式。
还应当进一步理解,在本发明说明书和所附权利要求书中使用的术语“和/或”是指相关联列出的项中的一个或多个的任何组合以及所有可能组合,并且包括这些组合。
实施例1
一种基于光固化成型的氧化铝陶瓷-树脂复合材料的制备方法
(1)制备具备连通孔隙的陶瓷基体
首先称量63.68g氧化铝陶瓷粉体、8.56g 1,6己二醇二丙烯酸酯、8.56g乙氧化季戍四醇四丙烯酸酯、0.17g光引发剂(2,4,6-三甲基苯甲酰基)、0.64g分散剂(KOS110)和30g氧化锆球磨球置于球磨罐中,然后使用行星球磨机以350r/min的转速球磨4h,制备混合均匀的固相含量为50vol%的氧化铝陶瓷浆料。在光固化成型打印机中导入陶瓷基体的模型,模型如图1所示,模型的孔隙截面的形状为圆形,孔隙的直径大小为100μm。设置打印的固化时间为1.5s,405nm的紫外光光强为9mW/cm2,切片的层厚为20μm。通过打印获得陶瓷坯体,然后进行脱脂烧结,具体工艺如下:将坯体置于空气脱脂炉中以0.5℃/min的升温速率升温至600℃,在升温过程中每升温150℃保温1h,在600℃保温3h,然后随炉冷却至室温。将脱脂样品置于马弗炉中于空气气氛下烧结,以10℃/min的升温速率升温至1200℃,然后以5℃/min的升温速率升温至1600℃,保温2h。接着以10℃/min降温至800℃,然后随炉冷却至室温。所制备陶瓷基体完全致密,实际孔径大小约为80μm,显气孔率为23%。
(2)树脂浸渗及固化
称量80g双酚A型环氧树脂,8g乙二胺,20g邻苯二甲酸二丁酯于烧杯中,在常温条件下,使用机械搅拌混合4h获得热固化的树脂混合液,该树脂混合液的粘度为0.3Pa·s。将烧结完成的陶瓷基体放入装有树脂混合液的烧杯中,然后置于常温的真空干燥箱中浸渗2h,真空度设置为0.01MPa;浸渗结束后,加热至140℃,保温固化4h。
(3)后续处理
取出上述固化完成后的样品,使用800目的砂纸打磨去除陶瓷基体固化的树脂,获得陶瓷-树脂复合材料。
通过上述方法制备的陶瓷-树脂复合材料内部含有微米尺度复合的树脂材料,其抗弯强度为542.32MPa,断裂韧性为8.3MPa。
实施例2
本实例中制备了一种氧化铝陶瓷-树脂复合材料,具体使用材料比例与工艺与实例1相同;不同之处为,光固化成型的陶瓷基体为图2模型,模型根据三周期极小曲面设计的多孔结构,使用的函数是doubleG曲线,频率3,偏移厚度3.3mm,孔隙为毫米级别。陶瓷基体的显气孔率为32%。该方法制备的氧化铝陶瓷-树脂复合材料抗弯强度为657.21MPa,断裂韧性为10.02MPa·m1/2.
实施例3
本实例中制备了一种氧化铝陶瓷-树脂复合材料,工艺步骤与与实例1相同;不同之处在于步骤(2)中,所用的树脂为水溶性酚醛树脂,固化过程的温度为160℃。通过上述方法制备的陶瓷-树脂复合材料内部含有微米尺度复合的树脂材料,其抗弯强度为520.12MPa,断裂韧性为8.9MPa·m1/2。
实施例4
一种基于光固化成型的氧化锆陶瓷-树脂复合材料的制备方法
(1)制备具备连通孔隙的陶瓷基体
首先称量93.60g 3Y-ZrO2陶瓷粉体(平均粒径0.5μm)、8.56g 1,6己二醇二丙烯酸酯、8.56g乙氧化季戍四醇四丙烯酸酯、0.17g光引发剂(2,4,6-三甲基苯甲酰基)、0.94g分散剂(KOS110)和30g氧化锆球磨球置于球磨罐中,然后使用行星球磨机以350r/min的转速球磨4h,制备混合均匀的固相含量为50vol%的氧化锆陶瓷浆料。在光固化成型打印中导入陶瓷基体的模型,模型如图2所示,根据三周期极小曲面设计的多孔结构,使用的函数是doubleG曲线,频率3,偏移厚度3.3mm,孔隙为毫米级别。设置打印的固化时间为2s,405nm的紫外光光强为12mW/cm2,切片的层厚为20μm。通过打印获得陶瓷坯体,然后进行脱脂烧结,具体工艺如下:将坯体置于空气脱脂炉中以0.5℃/min的升温速率升温至500℃,在升温过程中每升温100℃保温1h,在500℃保温3h,然后随炉冷却至室温。将脱脂样品置于马弗炉中于空气气氛下烧结,以10℃/min的升温速率升温至1200℃,然后以4℃/min的升温速率升温至1550℃,保温2h。接着以10℃/min降温至800℃,然后随炉冷却至室温。所制备陶瓷基体完全致密,显气孔率为40%。
(2)树脂浸渗及固化
称量60g季戊四醇四丙烯酸酯、20g1,6己二醇二丙烯酸酯,10g邻苯二甲酸二辛脂,1.5g2,4,6-三甲基苯甲酰基,于烧杯中,在常温条件下,使用机械搅拌混合2h获得光固化的树脂混合液,该树脂混合液的粘度为0.13Pa·s。将烧结完成的陶瓷基体放入装有树脂混合液的烧杯中,然后置于常温的真空干燥箱中浸渗2h,真空度设置为0.1MPa;浸渗完成后,将烧杯取出,使用光强为16mW/cm2紫外光照射树脂混合液1h,使树脂完全固化。
(3)后续处理
取出上述固化完成后的样品,使用800目的砂纸打磨去除陶瓷基体固化的树脂,获得陶瓷-树脂复合材料。
通过上述方法制备的氧化锆陶瓷-树脂复合材料内部为毫米尺度复合的树脂材料,且内部孔隙基于仿生微孔结构设计。其抗弯强度为700.32MPa,断裂韧性为12.1MPa·m1 /2。
在上述实施例中,对各个实施例的描述都各有侧重,某个实施例中没有详细描述的部分,可以参见其他实施例的相关描述。
显然,本领域的技术人员可以对本发明进行各种改动和变型而不脱离本发明的精神和范围。这样,尚且本发明的这些修改和变型属于本发明权利要求及其等同技术的范围之内,则本发明也意图包含这些改动和变型在内。
以上所述,仅为本发明的具体实施方式,但本发明的保护范围并不局限于此,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,可轻易想到各种等效的修改或替换,这些修改或替换都应涵盖在本发明的保护范围之内。因此,本发明的保护范围应以权利要求的保护范围为准。
Claims (10)
1.一种基于光固化成型的陶瓷-树脂复合材料的制备方法,其特征在于,包括:
步骤1,将陶瓷粉体、第一光固化树脂和光引发剂混合制成陶瓷浆料,基于所述陶瓷浆料,使用光固化成型打印机制备根据预设的结构图纸光固化成型具有连通孔结构的陶瓷坯体,依次对陶瓷坯体执行脱脂处理和烧结处理,获得陶瓷基体;
步骤2,将所述陶瓷基体浸渍在充满树脂混合液的容器中,使得所述树脂混合液浸渗到所述陶瓷基体的孔隙中,并将所述树脂混合液固化为树脂材料;
步骤3,清理所述陶瓷基体周围固化的树脂材料,获得陶瓷-树脂复合材料。
2.根据权利要求1所述的方法,其特征在于,所述步骤1中,采用球磨方式将陶瓷粉体、第一光固化树脂和光引发剂混合制成陶瓷浆料,其中,球磨时间为4-6h,球磨转速为200-350r/min,陶瓷浆料的固含量为40-60vol%。
3.根据权利要求1所述的方法,其特征在于,所述步骤1中,光固化成型的曝光时间为2-4s,紫外光光强为7-15mW/cm2。
4.根据权利要求1所述的方法,其特征在于,所述步骤1中,脱脂处理的工艺为空气脱脂,包括:以升温速率为0.5℃/min升温,每升温100℃保温1h,直至升至最高温度550-600℃,在最高温度保温6h;然后以0.5℃/min降温至200℃,最后随炉冷却;
所述步骤1中,烧结处理的工艺为无压烧结,包括:以5℃/min升温至1400-1650℃,保温2h;然后以5℃/min降温至800℃,最后随炉冷却。
5.根据权利要求1所述的方法,其特征在于,所述树脂混合液包括热固化树脂、塑化剂以及热引发剂,或者,所述树脂混合液包括第二光固化树脂、塑化剂以及光引发剂;所述热引发剂为胺类固化剂;所述光引发剂2,4,6-三甲基苯甲酰基-二苯基氧化膦、2,4,6-三甲基苯甲酰基以及二异丙基二氨基苯甲酰化物中的至少一种,所述塑化剂为邻苯二甲酸二丁酯、聚乙二醇以及2-羟基乙基丙烯酸三甲酯中的至少一种;所述热固化树脂为双酚A型环氧树脂、环氧树脂以及酚醛树脂中的至少一种;所述第二光固化树脂为季戊四醇四丙烯酸酯、三羟甲基丙烷三丙烯酸酯以及1,6-己二醇二丙烯酸酯中的至少一种。
6.根据权利要求5所述的方法,其特征在于,以质量份计,所述树脂混合液包括热固化树脂60-80份,塑化剂10-30份,热引发剂10-20份,所述树脂混合液固化过程的工艺参数包括固化温度为100-350℃,固化时间为0.5-4h;
或者,以质量份计,所述树脂混合液包括第二光固化树脂60-80份,塑化剂20-40份,光引发剂1-5份,所述树脂混合液固化过程的工艺参数包括照射时间为0.5-4h,紫外光光强为15-20mW/cm2。
7.根据权利要求1所述的方法,其特征在于,所述步骤2中,所述树脂混合液浸渍过程的工艺参数包括真空度为0.01-0.1MPa,浸渗时间为10-48h。
8.根据权利要求1所述的方法,其特征在于,所述陶瓷基体内部包括相互连通的孔,所述孔的孔径为微米级或者毫米级,所述孔的截面形状为圆形、方形、椭圆形和不规则形状中的至少一种。
9.一种陶瓷-树脂复合材料,其特征在于,由权利要求1-8任一项所述的方法制备,所述陶瓷-树脂复合材料的抗弯强度为500~700MPa,断裂韧性为6~20Pa·m1/2。
10.根据权利要求9所述的陶瓷-树脂复合材料,其特征在于,所述陶瓷-树脂复合材料包括陶瓷基体以及树脂,所述陶瓷基体包括氧化锆陶瓷或者氧化铝陶瓷中的至少一种;以体积分数计,陶瓷基体的含量为50-80%。
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