CN117303877A - 一种基于粘结剂喷射技术制备高性能结构陶瓷的方法 - Google Patents
一种基于粘结剂喷射技术制备高性能结构陶瓷的方法 Download PDFInfo
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- CN117303877A CN117303877A CN202311242263.9A CN202311242263A CN117303877A CN 117303877 A CN117303877 A CN 117303877A CN 202311242263 A CN202311242263 A CN 202311242263A CN 117303877 A CN117303877 A CN 117303877A
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- Compositions Of Oxide Ceramics (AREA)
Abstract
本发明公开了一种基于粘结剂喷射技术制备高性能结构陶瓷的方法，涉及增材制造技术领域。本发明先将陶瓷粉体和烧结助剂混合均匀，然后加入含有金属盐、硅溶胶、胶水的混合悬浮液，进行造粒制备粗粉；将所述粗粉用粘结剂喷射技术成型制坯；对坯体进行脱脂、烧结，制得陶瓷基芯。本发明利用具有高烧结活性的陶瓷粉体、烧结助剂粉体、金属盐化合物、硅溶胶和胶水制备微米级粗粉，然后通过粘结剂喷射工艺制备陶瓷打印样品，从而能够获得具有较高强度的打印坯体，并且坯体在脱脂后仍能保持较高强度，有利于高温烧结制备出具有高致密、高强度的结构陶瓷，解决了粘结剂喷射增材制造技术难以制备高密度高性能陶瓷的问题。
Description
技术领域
本发明涉及增材制造技术领域，尤其涉及一种基于粘结剂喷射技术制备高性能结构陶瓷的方法。
背景技术
结构陶瓷是具有耐高温、耐冲刷、耐腐蚀、高硬度、高强度、低蠕变速率等优异力学、热学、化学性能，常用于各种结构部件的先进陶瓷。用于制造结构陶瓷的材料例如氧化铝、氧化锆、氮化硅等，烧结成型后具有高强度和高硬度的特点。
增材制造技术为复杂形状陶瓷构件的制备提供了新方向。其中，粘结剂喷射增材制造(BJAM)是基于粉末床工艺，通过喷墨打印头逐层喷射粘结剂选区沉积在粉末床上，层层叠加形成零件生坯，并通过后续固化、脱脂、烧结过程，使其致密化并获得机械性能良好的零件。BJAM技术具有快速高效、低成本、无需额外支撑等特点，不仅具有较高的精度而且适合大型构件的制备以及批量化生产。
为了获得良好的铺粉效果，BJAM技术对粉体有较高的要求，例如高流动性，因此通常使用近球形粉体，粒径范围在10-200um。但是，先进陶瓷材料的粉体特性(粒径、比表面积等)对其烧结活性有很大影响。通常而言，粒径越小，比表面越大，烧结活性越高，烧结温度也越低。在高性能陶瓷制备过程中通常采用亚微米、纳米级粉体的原材料，提供足够的烧结活性保证材料完全致密化。而BJAM所使用的10-200um粒径的陶瓷粉体，会使得粉体的烧结活性严重降低，该粒径范围的粉体通常用来做多孔陶瓷，隔热材料等，导致采用BJAM技术制备高密度高性能的先进陶瓷十分困难。另外，基于粉床工艺，粉床密度等多方面的影响，例如粉体特性(粒径大小、分布、形貌等)，铺粉工艺(铺粉方式、厚度、速度等)，几乎没有外力作用的粉床依靠自然堆积实现，粉体颗粒之间接触点较少，而且孔隙较大，不利于高性能结构陶瓷的烧结。
发明内容
本发明所要解决的技术问题是如何采用粘结剂喷射成型技术制备高密度、高强度的结构陶瓷。
为了解决上述问题，本发明提出以下技术方案：
一方面，本发明提出一种基于粘结剂喷射技术制备高性能结构陶瓷的方法，包括以下步骤：
S1、按质量份计，先将陶瓷粉体80～99份和烧结助剂1～20份混合均匀，然后向混合粉体中加入含有金属盐20～30份、硅溶胶20～30份、胶水20～30份混合悬浮液，进行造粒制备粗粉，粗粉粒径为0.1um～150um，优选0.1-60um；
S2、将所述粗粉用粘结剂喷射技术成型制坯；
S3、对坯体进行脱脂、烧结，制得陶瓷基芯；
所述陶瓷粉体的粒径范围为1nm～10um；所述金属盐选自碱土金属硝酸盐和/或稀土金属硝酸盐。
所述陶瓷粉体的粒径范围为1nm～10um，优选100nm～1um，在此粒径范围下，陶瓷粉体具有更高烧结活性。
需要说明的是，所述混合悬浮溶液是将金属盐预先溶于溶剂中，然后加入硅溶胶以及胶水混合制得，所用的溶剂可以是无水乙醇。
本发明的造粒方式优选挤压搅拌造粒，原理见图2，具体是将陶瓷粉体和烧结助剂混合后，在对混合粉体进行挤压搅拌时，从喷头处按需喷出含有金属盐、硅溶胶、胶水的混合悬浮液，随后烘干得到粗粉。这种造粒方式使得混合悬浮液的加入在造粒时不会影响粉体原料的堆积情况，同时，混合悬浮液中的成份有利于提高粗粉的密度，进而提高坯体的密度。坯体密度越高，其烧结得到的陶瓷密度也越高。进一步地，在粘结剂喷射打印时，粘结剂喷射胶水进入粉床后与粗粉中的硅溶胶和金属盐混合，粘结剂喷射胶水对粉床浸润有助于硅溶胶和金属盐均匀地对坯体的孔隙进行二次填充，在脱脂后金属盐会分解为金属氧化物并形成壳核结构以及晶桥，强化了粉体原料之间的固体桥联，保证了脱脂后坯体的强度，并且形成的坯体内部结构较为均匀，有利于烧结得到致密的结构陶瓷。
其进一步地技术方案为，所述陶瓷粉体为氧化铝、氧化锆、氮化硅、氮化铝中的至少一种。
其进一步地技术方案为，所述金属盐选自Mg的硝酸盐化合物、Al的硝酸盐化合物、Zr的硝酸盐化合物、Ca的硝酸盐化合物、Y的硝酸盐化合物、Ce的硝酸盐化合物、Eu的硝酸盐化合物、La的硝酸盐化合物、Lu的硝酸盐化合物中的一种或多种。
其进一步地技术方案为，所述烧结助剂选自碱土金属氧化物和/或稀土金属氧化物。
其进一步地技术方案为，所述烧结助剂选自MgO、Al2O3、ZrO2、CaO、SiO2、Cr2O3、Y2O3、La2O3、Ce2O3、Sm2O3、Eu2O3、Gd2O3、Lu2O3中的一种或多种。
其进一步地技术方案为，所述烧结助剂的粒径范围为1nm～10um，优选范围100nm～1um。
其进一步地技术方案为，所述硅溶胶中的SiO2质量分数量为1～50％，优选15％～30％，SiO2的平均粒径范为1nm～500nm，优选10nm～150nm。
其进一步地技术方案为，所述胶水为粘接固化胶水，可选自环氧树脂类胶水、呋喃树脂类胶水、丙烯酸酯类胶水、酚醛类胶水、聚乙烯醇胶水、纤维素胶水、硅酸钠胶水中的一种或多种，本领域技术人员也可选用其他胶水达到类似的效果。
其进一步地技术方案为，所述步骤S2中，铺粉厚度为60um～200um。本领域技术人员可通过优化打印参数(铺粉速度、喷胶量等)保证不出现推件、层移、变形等问题，获得形状和精度良好的打印坯体。
需要说明的是，本发明中，脱脂是指去除打印体中的有机物，根据所含有机物的受热分解情况，其脱脂温度应在300-600℃左右，脱脂方法不限于一步空气脱脂、真空和空气两步脱脂等。对脱脂后的样品进行烧结，烧结温度在1300-1900℃，从而获得高致密、高性能的陶瓷，烧结温度应根据陶瓷材料的种类来确定。本发明中，脱脂和烧结为陶瓷材料的常规制备工艺，本领域技术人员可根据具体陶瓷材料采用合适设备以及烧结工艺进行烧结，例如氧化铝、氧化锆陶瓷材料可采用马弗炉进行烧结，氮化硅陶瓷材料可采用气氛炉、气压炉等进行烧结，但不局限于这几种。
另一方面，本发明提供一种粘接剂喷射制得的结构陶瓷基芯，由所述的基于粘结剂喷射技术制备高性能结构陶瓷的方法制得。
与现有技术相比，本发明所能达到的技术效果包括：
本发明利用具有高烧结活性的陶瓷粉体、烧结助剂粉体、金属盐化合物、硅溶胶和胶水制备微米级粗粉，然后通过粘结剂喷射工艺制备陶瓷打印样品，从而能够获得具有较高强度的打印坯体，并且坯体在脱脂后仍能保持较高强度，有利于高温烧结制备出具有高致密、高强度的结构陶瓷。本发明利用高烧结活性陶瓷粉体原料、硅溶胶中的纳米二氧化硅、烧结助剂以及金属盐分解的纳米氧化物的共同作用，通过液相烧结的方式来提高粘结剂喷射坯体的烧结性能，从而获得高密度、高强度的打印陶瓷坯体，并且烧结体的密度越高，其力学性能越优，解决了粘结剂喷射增材制造技术难以制备高密度高性能陶瓷的问题。
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1制备陶瓷粗粉及粘接剂喷射陶瓷的工艺流程示意图；
图2为本发明实施例1制备陶瓷粗粉时使用的挤压搅拌造粒机示意图，图中可看出，当陶瓷混合粉体在挤压板高速搅拌作用时，混合悬浮液通过喷头按需喷出，再经过烘干程序获得粗粉。
具体实施方式
下面将对实施例中的技术方案进行清楚、完整地描述。显然，以下将描述的实施例仅仅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，在此本发明实施例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实施例。如在本发明实施例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。
实施例1
本实施例提供一种基于粘结剂喷射技术制备高性能结构陶瓷的方法，其中，所用的粉体原料为纳米氧化铝粉体，中粒径为200nm。烧结助剂为氧化镁，中粒径为50nm。
混合悬浮液中：金属盐为六水合硝酸钇；硅溶胶为二氧化硅含量29～31％，平均粒径为10-16nm的硅溶胶；胶水为质量分数为5％的聚乙烯醇水溶液；混合悬浮液中的溶剂为无水乙醇。
参见图1，本实施例采用粘结剂喷射技术制备高性能结构陶瓷的方法，包括以下步骤：
S1：按质量份计，取氧化铝99份，氧化镁1份，以无水乙醇为介质，加入氧化铝磨球，球磨混合12小时，然后使用旋转蒸发仪干燥后获得混合均匀的混合粉体；
按质量份计，取六水合硝酸钇20份、无水乙醇20份、硅溶胶20份和聚乙烯醇水溶液20份混合，搅拌超声混合30分钟，获得混合均匀的混合悬浮液。
S2：参见图2，采用挤压搅拌造粒的方式进行造粒，向混合粉体中加入混合悬浮液，悬浮液加入量为粉体质量的10％，随后烘干，使用筛网去除大于74um的颗粒，得到粗粉。测量该粗粉的松装密度和振实密度。
S3：使用商用粘结剂喷射打印机以及商用胶水打印零件，铺粉厚度设置在100um，并优化打印参数(铺粉速度、喷胶量等)，最后打印出形状和精度良好的氧化铝打印体。
S4：使用马弗炉对打印样件进行脱脂，脱脂工艺为空气脱脂，600℃保温2小时，测量脱脂后坯体的抗压强度；使用马弗炉对脱脂坯体进行烧结，烧结工艺为1600℃烧结2小时，烧结后获得高致密、高性能的氧化铝结构陶瓷。测量烧结件的抗弯强度。
实施例2
本实施例与实施例1的不同之处在于，混合悬浮液中金属盐为六水合硝酸钇和硝酸锆。本实施例混合悬浮液的组成为六水合硝酸钇10份、硝酸锆10份、无水乙醇20份、硅溶胶20份和聚乙烯醇水溶液20份。其他参数和制备工艺与实施例1相同。
实施例3
本实施例与实施例1的不同之处在于，所用的粉体原料为氧化铝，中粒径为200nm。烧结助剂为氧化镁和氧化锆，中粒径分别为50nm和50nm。其他参数和制备工艺与实施例1相同。
对比例1
本对比例所用的粉体原料仅为氧化铝粉体，中粒径为45um，以此原料粉体作为打印用粗粉，测量其松装密度和振实密度。然后使用商用粘结剂喷射打印机以及商用胶水打印零件，铺粉厚度设置在100um，并优化打印参数(铺粉速度、喷胶量等)，最后打印出氧化铝打印体。进一步使用马弗炉对打印样件进行脱脂，脱脂工艺为空气脱脂，600℃保温2小时，测量脱脂后坯体的抗压强度；使用马弗炉对脱脂坯体进行烧结，烧结工艺为1600℃烧结2小时，得到烧结件。测量烧结件的抗弯强度。
对比例2
本对比例所用的粉体原料为氧化铝，中粒径为45um。烧结助剂为氧化镁，中粒径50nm；二氧化硅，中粒径为50nm。
本对比例的制备方法如下：
按质量份计，取氧化铝98份，氧化镁1份，二氧化硅1份，以无水乙醇为介质，加入氧化铝磨球，滚筒球磨混合12小时，使用旋转蒸发仪干燥后获得均匀混合的混合粉体。以此混合粉体作为打印用粗粉，测量其松装密度和振实密度。
使用商用粘结剂喷射打印机以及商用胶水打印零件，铺粉厚度设置在100um，并优化打印参数(铺粉速度、喷胶量等)，最后打印出氧化铝打印体。进一步使用马弗炉对打印样件进行脱脂，脱脂工艺为空气脱脂，600℃保温2小时，测量脱脂后坯体的抗压强度；使用马弗炉对脱脂坯体进行烧结，烧结工艺为1600℃烧结2小时，得到烧结件。测量烧结件的抗弯强度。
对比例3
本对比例所用的粉体原料仅为氧化铝粉体，中粒径为200nm，以此原料粉体作为打印用粗粉，测量其松装密度和振实密度。然后使用马弗炉进行松装烧结(将混合粉体倒入坩埚内，不加施加压力，不振实)，烧结工艺为1600℃烧结2小时，烧结后获得氧化铝烧结件。测量烧结件的密度。
需要说明的是，本对比例中，采用的原料粉体为纳米粉体，具有非常差的流动性，无法完成在粘接喷射打印机上进行铺粉，因此，本对比例使用松装烧结进行模拟。
对比例4
本对比例所用的粉体原料为氧化铝，中粒径为200nm。烧结助剂为烧结助剂为氧化镁，中粒径50nm；二氧化硅，中粒径为50nm。
本对比例的混合悬浮液中不含硅溶胶，混合悬浮液的组成为六水合硝酸钇20份、无水乙醇20份和聚乙烯醇水溶液20份。
本对比例的制备方法如下：
按质量份计，取氧化铝98份，氧化镁1份，二氧化硅1份，以无水乙醇为介质，加入氧化铝磨球，滚筒球磨混合12小时，使用旋转蒸发仪干燥后获得均匀的混合粉体。
采用挤压搅拌造粒的方式进行造粒，向混合粉体中加入混合悬浮液，悬浮液加入量为粉体质量的10％，随后烘干，使用筛网去除大于74um的颗粒，得到粗粉。测量该粗粉的松装密度和振实密度。
使用商用粘结剂喷射打印机以及商用胶水打印零件，铺粉厚度设置在100um，并优化打印参数(铺粉速度、喷胶量等)，最后打印出氧化铝打印体。进一步使用马弗炉对打印样件进行脱脂，脱脂工艺为空气脱脂，600℃保温2小时，测量脱脂后坯体的抗压强度；使用马弗炉对脱脂坯体进行烧结，烧结工艺为1600℃烧结2小时，得到烧结件。测量烧结件的抗弯强度。
对比例5
本对比例与实施例1的不同之处在于，混合悬浮液中不含金属盐六水合硝酸钇、不含硅溶胶。本对比例混合悬浮液的组成为无水乙醇20份和聚乙烯醇水溶液20份。其他参数和实施例1相同。
对比例6
本对比例与实施例1的不同之处在于，混合悬浮液中不含硅溶胶。本实施例混合悬浮液的组成为六水合硝酸钇20份、无水乙醇20份和聚乙烯醇水溶液20份。其他参数和制备工艺与实施例1相同。
对比例7
本对比例与实施例1的不同之处在于，混合悬浮液中不含金属盐六水合硝酸钇。本实施例混合悬浮液的组成为硅溶胶20份、无水乙醇20份和聚乙烯醇水溶液20份。其他参数和制备工艺与实施例1相同。
对本发明实施例1～3以及对比例1～7中的相关数据进行比较，见表1。
表1本发明实施例1与对比例1～7中的实验相关数据
表1中，对比例1、2、5、7打印件脱脂后基本无强度，对比例3、4未进行打印，以上不再做抗压强度，用/标出。
上述表1结果说明，实施例1-3通过优化陶瓷原料粉体粒径，加入金属盐和硅溶胶对陶瓷粉体重新造粒，制备得到的粗粉可以实现较高的粉床填充密度，并通过液相烧结法促进烧结，获得高致密度、高强度的氧化铝陶瓷；同时，采用本发明方法，粗粉可以采用粘接剂技术制坯，脱脂后具有一定的抗压强度，这是本发明独特的优势，有利于生产制造出高性能的结构陶瓷。
对比例1～2的陶瓷原料粉体粒径较粗，虽然能够获得较高的松装密度和振实密度，但是粒径45um的球形氧化铝粉体的烧结性能太低，即使加入烧结助剂也远低于实施例1的相对密度。
对比例3采用了200nm氧化铝粉体原料，但是其未加入混合悬浮液重新对粉体原料进行造粒，导致打印用的粉体松装密度和振实密度较低，烧结后的密度也较低，与实施例1的相对密度相差较大。
对比例4以纳米二氧化硅替代混合悬浮液中的硅溶胶，制备工艺与实施例1相同，虽然造粒的粉体能够具有较高的松装密度和振实密度，但不如实施例1，烧结后的陶瓷密度、强度均不如实施例1。
在对比例5～7中，混合悬浮液只添加了金属盐或者硅溶胶或者不含金属盐及硅溶胶，重新造粒得到的粗粉松装密度和振实密度均低于实施例1，并且烧结后的密度也较低。
以上实施例仅以制备氧化铝陶瓷为例进行说明本发明利用具有高烧结活性的陶瓷粉体、烧结助剂粉体、金属盐化合物、硅溶胶和胶水制备微米级粗粉，采用粘接剂喷射技术能够获得具有较高抗压强度的坯体，经烧结之后得到高性能的陶瓷，本领域技术人员采用氧化锆、氮化硅或氮化铝陶瓷粉体进行制备也能获得相类似的效果。
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。
以上所述，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)
1.一种基于粘结剂喷射技术制备高性能结构陶瓷的方法，其特征在于，包括以下步骤：
S1、按质量份计，先将陶瓷粉体80～99份和烧结助剂1～20份混合均匀，然后向混合粉体中加入含有金属盐20～30份、硅溶胶20～30份、胶水20～30份的混合悬浮液，进行造粒制备粗粉，粗粉粒径为0.1um～150um；
S2、将所述粗粉用粘结剂喷射技术成型制坯；
S3、对坯体进行脱脂、烧结，制得陶瓷基芯；
所述陶瓷粉体的粒径范围为1nm～10um，所述金属盐选自碱土金属硝酸盐和/或稀土金属硝酸盐。
2.如权利要求1所述的基于粘结剂喷射技术制备高性能结构陶瓷的方法，其特征在于，所述陶瓷粉体为氧化铝、氧化锆、氮化硅、氮化铝中的至少一种。
3.如权利要求1所述的基于粘结剂喷射技术制备高性能结构陶瓷的方法，其特征在于，所述金属盐选自Mg的硝酸盐化合物、Al的硝酸盐化合物、Zr的硝酸盐化合物、Ca的硝酸盐化合物、Y的硝酸盐化合物、Ce的硝酸盐化合物、Eu的硝酸盐化合物、La的硝酸盐化合物、Lu的硝酸盐化合物中的一种或多种。
4.如权利要求1所述的基于粘结剂喷射技术制备高性能结构陶瓷的方法，其特征在于，所述烧结助剂选自碱土金属氧化物和/或稀土金属氧化物。
5.如权利要求4所述的基于粘结剂喷射技术制备高性能结构陶瓷的方法，其特征在于，所述烧结助剂选自MgO、Al2O3、ZrO2、CaO、SiO2、Cr2O3、Y2O3、La2O3、Ce2O3、Sm2O3、Eu2O3、Gd2O3、Lu2O3中的一种或多种。
6.如权利要求1所述的基于粘结剂喷射技术制备高性能结构陶瓷的方法，其特征在于，所述烧结助剂的粒径范围为1nm～10um。
7.如权利要求1所述的基于粘结剂喷射技术制备高性能结构陶瓷的方法，其特征在于，所述硅溶胶中的SiO2质量分数量为1～50％，SiO2的平均粒径为1nm～500nm。
8.如权利要求1所述的基于粘结剂喷射技术制备高性能结构陶瓷的方法，其特征在于，所述胶水选自环氧树脂类胶水、呋喃树脂类胶水、丙烯酸酯类胶水、酚醛类胶水、聚乙烯醇胶水、纤维素胶水、硅酸钠胶水中的一种或多种。
9.如权利要求1所述的基于粘结剂喷射技术制备高性能结构陶瓷的方法，其特征在于，所述步骤S2中，铺粉厚度为60um～200um。
10.一种粘接剂喷射制得的结构陶瓷基芯，其特征在于，由权利要求1-9任一项所述的基于粘结剂喷射技术制备高性能结构陶瓷的方法制得。
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