CN117383916A - 一种可溶性陶瓷芯、制备方法与应用 - Google Patents
一种可溶性陶瓷芯、制备方法与应用 Download PDFInfo
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- CN117383916A CN117383916A CN202311224186.4A CN202311224186A CN117383916A CN 117383916 A CN117383916 A CN 117383916A CN 202311224186 A CN202311224186 A CN 202311224186A CN 117383916 A CN117383916 A CN 117383916A
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- Molds, Cores, And Manufacturing Methods Thereof (AREA)
Abstract
本发明涉及一种可溶性陶瓷芯、制备方法与应用，属于快速铸造相关技术领域。本发明的制备方法包括以下步骤：(1)将陶瓷粉和可溶性盐混合均匀，运用微滴喷射粘结成型工艺打印出陶瓷芯初坯，经过固化、浸渗以及烘干后得到陶瓷芯坯体；(2)将陶瓷坯体放入高温烧结炉中进行烧结，随炉冷却后得到可溶性陶瓷芯。本发明通过将陶瓷粉和可溶性盐混合均匀，运用微滴喷射粘结成型工艺制备可溶性陶瓷芯，操作简单、生产效率高、成本低，适合成型大型复杂结构陶瓷芯，本发明制备的陶瓷芯具有良好的可溶性，在浇注结束后十分便于从铸件中去除。
Description
技术领域
本发明属于增材制造相关技术领域，更具体地，涉及一种可溶性陶瓷芯、制备方法与应用。
背景技术
随着国内航空航天、武器装备等领域的快速发展，对大型复杂形状构件的制造技术提出了新的要求，包括结构功能统一、整体铸造、薄壁、高精度、可靠性等。其中部分构件结构复杂，存在大尺寸的空腔结构，一部分铸件的内腔具有细小或不规则的管路的复杂结构，或内腔通过挂壳技术无法实现干燥硬化，又难以进行机械加工时，如叶轮、回油管路、引气弯管等，此时仅依靠精密铸造型壳已不能满足复杂铸件的铸造需求，必须借助陶瓷芯与型壳相互配合才能生产出具有复杂内腔的铸件。然而，制造陶瓷芯的传统技术，如凝胶铸造、注射成型和热压，普遍存在一些缺点，包括难以制造具有复杂几何形状的陶瓷芯，制备周期长，以及难以在低产量下平衡模具设计的成本等。因此，如何快速制备复杂结构陶瓷芯，降低生产成本是目前急需解决的问题。
增材制造技术是指在计算机的控制下，将零件的3D模型进行切片，并逐层打印，最终形成完整零件的过程。将增材制造技术应用到陶瓷型壳的生产过程中可以突破传统工艺中面临的周期长、成本高、工艺复杂且存在局限性等问题，有利于促进各行业的进一步发展。目前可用于陶瓷型壳成型制备的增材制造技术主要包括：光固化成型(SLA)技术、激光选区烧结(SLS)技术、微滴喷射粘结成型(BJ)技术等等。相比较SLA和SLS技术，BJ技术制造陶瓷芯具有高效率、低成本和优异性能的综合优势。其一，BJ技术采用阵列式喷头喷射材料，属于面成形，其制造效率是SLA和SLS的数十到数百倍；其次，BJ技术属于粘结成形，无热源和热变形，在制造过程中无应力和开裂问题，具有广阔的应用前景。
为保证铸件内部可以形成良好的空腔结构，陶瓷芯必须具有良好的化学稳定性和高温抗蠕变性能，常用的陶瓷芯制备材料主要有SiO2和Al2O3两种，此外近些年ZrO2以及Y2O3等材料也被逐渐用于陶瓷芯的制备中。铸件浇注成功后，还需要将陶瓷芯从铸件中去除，使内部空腔腔完全裸露，才能充分发挥空腔的功能，但上述材料制备出的陶瓷芯在后续脱芯过程中存在着一定难度。以浓碱液作脱芯介质，在高温高压下进行化学腐蚀反应是目前常用的脱芯方法，但这种方法存在着如易对铸件表面形成腐蚀、复杂弯曲型芯去除效果不理想等问题，脱出技术成为制约陶瓷芯使用的一大瓶颈。因此，急需开发一种可溶性陶瓷芯材料及其制备方法，解决上述制备技术和陶瓷芯材料存在的问题，满足工业生产需求。
发明内容
针对现有技术的以上缺陷或改进需求，本发明提供了一种基于微滴喷射粘结成型的可溶性陶瓷芯及其制备方法与应用，采用陶瓷粉骨料与可溶性盐干态粘结剂混合作为陶瓷芯材料，高温下陶瓷骨料与熔融状态下的盐紧密烧结在一起，随炉冷却后得到可溶性陶瓷芯。浇注后将铸件放入水中，陶瓷芯中的盐遇水发生溶解，陶瓷芯便会发生溃散，轻松与铸件分离，操作简单，极大简化了后期脱芯工序，且对铸件本身不会造成损害。
根据本发明第一方面，提供了一种可溶性陶瓷芯的制备方法，包括以下步骤：
(1)将陶瓷粉骨料与干态粘结剂均匀混合后形成混合粉料，采用微滴喷射粘结成型工艺将所述混合粉料制成陶瓷芯初坯，然后对所述陶瓷芯初坯进行加热固化、浸渗和干燥，得到陶瓷芯坯体；所述干态粘接剂为可溶性盐；
(2)将步骤(1)得到的陶瓷芯坯体进行烧结，随炉冷却后即得到所述可溶性陶瓷芯。
优选地，步骤(1)中，所述微滴喷射粘结成型工艺中的打印参数为：打印层高0.05mm～0.20mm，粘接剂饱和度80％～160％；所述加热固化的温度为180℃～210℃，时间为3h～6h。
优选地，步骤(1)中，所述陶瓷粉骨料为石英、氧化铝、氧化锆、氧化钇中的一种或几种的混合物；所述干态粘结剂为氯化盐、硫酸盐、硅酸盐、磷酸盐、偏磷酸盐中的一种或几种的混合物；所述的陶瓷粉骨料和所述干态粘结剂的粒径为325目～1000目。
优选地，步骤(1)中，所述的混合粉料中，所述干态粘结剂所占质量分数为15％～50％。
优选地，步骤(1)中，所述浸渗使用的浸渗液为醇基浸渗液，所述醇基浸渗液为纳米SiO2醇基分散液、纳米ZrO2醇基分散液或纳米TiO2醇基分散液中的至少一种，浸渗时间为30s～3min，浸渗方式为常压浸渗或者真空浸渗，真空浸渗时真空度为0～50KPa，质量分数为10％～40％；所述浸渗液用于渗透进陶瓷芯坯体的孔隙中，使其在烧结过程中可保持形状完整，避免坯体坍塌。
优选地，步骤(2)中，所述烧结分为两个阶段，分别为在650℃～800℃下烧结1h～3h，然后在1100℃～1500℃下烧结1h～3h，烧结过程中升温速率为2～5℃/min。
根据本发明另一方面，提供了任一项所述方法制备得到的可溶性陶瓷芯。
根据本发明另一方面，本发明还提供了上述可溶性陶瓷芯在精密铸造中的应用。
优选地，所述可溶性陶瓷芯与型壳相互配合，用于空腔结构件的精密铸造。
优选地，将浇注完成后的构件放入水中，陶瓷芯遇水发生反应会开裂溃散，与结构件分离，形成空腔结构件。
总体而言，通过本发明所构思的以上技术方案与现有技术相比，主要具备以下的技术优点：
(1)本发明的方法采用陶瓷粉骨料与可溶性盐干态粘结剂混合作为陶瓷芯材料，高温烧结过程中陶瓷骨料与熔融状态下的盐紧密烧结在一起，随炉冷却后得到可溶性陶瓷芯，浇注后将铸件放入水中，陶瓷芯中的盐遇水发生溶解，陶瓷芯便会发生溃散，轻松与铸件分离；相对于纯SiO2、Al2O3、和Y2O3等材料制备的陶瓷芯，本发明制备的可溶性陶瓷芯在脱模时更省时省力，不易对铸件表面形成腐蚀，其为复杂弯曲型芯时的去除效果更加理想、工艺上操作更简单，且极大简化了后期脱芯工序，对铸件本身不会造成损害；本发明的制备方法可以解决传统工艺在成型大型复杂结构陶瓷芯时的局限性，缩短生产周期，降低生产成本，有巨大的发展潜力。
(2)本发明采用优选的微滴喷射粘结成型工艺制备陶瓷芯，可以解决传统工艺在成型大型复杂结构陶瓷芯时的局限性，缩短生产周期，降低生产成本，满足社会市场的生产需求，相比较于SLA和SLS技术，本发明优选的微滴喷射粘结成型工艺属于面成形，其制造效率是SLA和SLS的数十到数百倍，其次无热源和热变形，在制造过程中无应力和开裂问题，具有广阔的应用前景。
(3)本发明优选的浸渗工艺可以使得陶瓷芯坯体在高温烧结过程中保持形状完整，避免坯体坍塌，保障烧结质量。
附图说明
图1是本发明可溶性陶瓷芯的制备方法的流程示意图。
图2是本发明实施例1制备的陶瓷芯样品实物图。
图3是本发明实施例1制备陶瓷芯样品在水中不同时间下的溃散图。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合附图及实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅用以解释本发明，并不用于限定本发明。此外，下面所描述的本发明各个实施方式中所涉及到的技术特征只要彼此之间未构成冲突就可以相互组合。
如图1所示，一种基于微滴喷射粘结成型的可溶性陶瓷芯的制备方法，该方法主要包括以下步骤：
(1)将陶瓷粉骨料与可溶性盐干态粘结剂混合均匀放入粉缸中，导入陶瓷芯三维结构模型并调整打印参数，随后打印出陶瓷芯初坯；
(2)将打印好的初坯连同粉床放入烘干箱中加热固化；
(3)将固化后的坯体从粉床中取出，清除干净粉末进行溶胶浸渗，随后放入烘干箱中低温干燥；
(4)将步骤(3)得到的陶瓷芯坯体进行烧结，随炉冷却后即得到所述可溶性陶瓷芯。
进一步地，在步骤(1)中，所述陶瓷粉骨料为石英、氧化铝、氧化锆、氧化钇等粉料的一种或几种的混合物。
进一步地，在步骤(1)中，所述可溶性盐干态粘结剂为氯化盐、硫酸盐、硅酸盐、磷酸盐、偏磷酸盐等其中一种或几种的混合物。
进一步地，在步骤(1)中，所述的混合粉料中，可溶性盐干态粘结剂所占比例在15％～50％。
进一步地，在步骤(1)中，所述的陶瓷粉骨料和可溶性盐干态粘结剂的粒径为325目～1000目；微滴喷射粘结成型工艺所使用的粘结剂为酚醛树脂；打印参数为：打印层高0.05mm～0.20mm，粘接剂饱和度80％～160％。
进一步地，步骤(4)中，所述烧结分为两个阶段，分别为在650℃～800℃下烧结1h～3h，然后在1100℃～1500℃下烧结1h～3h，烧结过程中升温速率为2～5℃/min。
进一步地，步骤(2)中，所述加热固化的温度为180℃～210℃，时间为3h～6h。
进一步地，步骤(3)中，所述浸渗使用的浸渗液为醇基浸渗液，质量分数为10％～40％；所述浸渗液用于渗透进陶瓷芯坯体的孔隙中，使其在高温烧结过程中可保持形状完整，避免坯体坍塌。
进一步地，所述浸渗液为纳米SiO2醇基分散液、纳米ZrO2醇基分散液或纳米TiO2醇基分散液中的至少一种，浸渗时间为30s～3min，浸渗方式为常压浸渗或者真空浸渗，真空浸渗时真空度为0～50KPa。
本发明还提供了一种可溶性陶瓷芯，所述可溶性陶瓷芯是采用如上所述的可溶性陶瓷芯的制备方法制备而成的。
在实际增材制造中，将所述可溶性陶瓷芯与型壳相互配合，用于空腔结构件的精密铸造。将浇注完成后的结构件放入水中，陶瓷芯遇水发生反应会开裂溃散，与结构件分离，结构件便可获得目标形状的空腔。
以下结合几个具体实施例来对本发明进行进一步的详细说明。
实施例1
本发明实施例1提供的可溶性陶瓷芯的制备方法主要包括以下步骤：
S1，将1000目的石英和氯化钠混合均匀，其中氯化钠添加比例为15％，混合后的粉末在80℃下干燥12h，取出后对粉末进行过筛。将筛好的混合粉末铺满供粉缸，在计算机中导入陶瓷芯的三维结构模型，并调整3D打印机的各项打印参数。随后开始打印，喷头、供粉缸和工作缸按照设置好的程序运行，直至打印过程结束。其中，所述3D打印设备打印参数为：打印层高0.05mm，粘结剂饱和度80％。
S2，打印结束后，将打印好的陶瓷芯坯体连同粉床放入烘干箱中，在180℃下加热固化3h。冷却后将陶瓷芯坯体从粉床中取出，并清除干净其周围多余的粉末。随后，将陶瓷芯坯体浸入10％纳米ZrO2醇基分散液中，在常压下浸渗3min后取出，随后放入70℃的烘干箱中干燥6h。
S3，将浸渗后的陶瓷坯体放入坩埚中，并用球形氧化铝颗粒完全填埋，随后将其放入马弗炉中进行高温烧结。其烧结曲线按照650℃烧结1h，1100℃烧结1h，升温速率为2℃/min的工艺参数进行烧结，最后，随炉冷却得到可溶性陶瓷芯，如图2所示。
实施例2
本发明实施例2提供的可溶性陶瓷芯的制备方法主要包括以下步骤：
S1，将800目的氧化铝和硫酸钠混合均匀，其中硫酸钠添加比例为30％，混合后的粉末在90℃下干燥10h，取出后对粉末进行过筛。将筛好的混合粉末铺满供粉缸，在计算机中导入陶瓷芯的三维结构模型，并调整3D打印机的各项打印参数。随后开始打印，喷头、供粉缸和工作缸按照设置好的程序运行，直至打印过程结束。其中，所述3D打印设备打印参数为：打印层高0.12mm，粘结剂饱和度120％。
S2，打印结束后，将打印好的陶瓷芯坯体连同粉床放入烘干箱中，在200℃下加热固化5h。冷却后将陶瓷芯坯体从粉床中取出，并清除干净其周围多余的粉末。随后，将陶瓷芯坯体浸入30％纳米SiO2醇基分散液中，随后放入真空浸渗装置中在25KPa的真空度下浸渗2min后取出，随后放入80℃的烘干箱中干燥5h。
S3，将浸渗后的陶瓷坯体放入坩埚中，并用球形氧化铝颗粒完全填埋，随后将其放入马弗炉中进行高温烧结。其烧结曲线按照700℃烧结1h，1300℃烧结1.5h，升温速率为3℃/min的工艺参数进行烧结，最后，随炉冷却得到可溶性陶瓷芯。
实施例3
本发明实施例3提供的可溶性陶瓷芯的制备方法主要包括以下步骤：
S1，将325目的氧化锆和磷酸三钾混合均匀，其中磷酸三钾添加比例为50％，混合后的粉末在100℃下干燥12h，取出后对粉末进行过筛。将筛好的混合粉末铺满供粉缸，在计算机中导入陶瓷芯的三维结构模型，并调整3D打印机的各项打印参数。随后开始打印，喷头、供粉缸和工作缸按照设置好的程序运行，直至打印过程结束。其中，所述3D打印设备打印参数为：打印层高0.20mm，粘结剂饱和度160％。
S2，打印结束后，将打印好的陶瓷芯坯体连同粉床放入烘干箱中，在210℃下加热固化6h。冷却后将陶瓷芯坯体从粉床中取出，并清除干净其周围多余的粉末。随后，将陶瓷芯坯体浸入40％纳米TiO2醇基分散液中，随后放入真空浸渗装置中在50KPa的真空度下浸渗30s后取出，随后放入90℃的烘干箱中干燥6h。
S3，将浸渗后的陶瓷坯体放入坩埚中，并用球形氧化铝颗粒完全填埋，随后将其放入马弗炉中进行高温烧结。其烧结曲线按照800℃烧结3h，1500℃烧结3h，升温速率为5℃/min的工艺参数进行烧结，最后，随炉冷却得到可溶性陶瓷芯。
应用实施例
随着涡轮发动机进口燃气温度的不断提高，单纯依靠提高材料的承温能力和采用隔热措施已无法满足服役需求，因此，通过复杂气冷内腔结构改善涡轮叶片散热能力已成为先进发动机制造的关键，而陶瓷型芯是铸造具有复杂气冷内腔结构叶片的核心部件。以制备涡轮叶片为例，首先按照上述具体实施例1中的方法制备得到可溶性涡轮叶片型芯，将型芯与型壳配合好放置在压力铸造设备中，用坩埚将熔融的钛合金液倒入型壳上方的浇口中，然后加压使金属液充满型壳。待冷却后，将浇注后的铸件取出并放入水中充分浸泡，如图3所示，其中图3中的(a)、图3中的(b)、图3中的(c)所示分别为铸件浸泡1min、2min、3min的实物图。5min后，陶瓷芯完全溃散，如图3中的(d)所示，从水中取出铸件，清洁干净后即可得到具有空心结构的涡轮空心叶片。
本领域的技术人员容易理解，以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。
Claims (10)
1.一种可溶性陶瓷芯的制备方法，其特征在于，包括以下步骤：
(1)将陶瓷粉骨料与干态粘结剂均匀混合后形成混合粉料，采用微滴喷射粘结成型工艺将所述混合粉料制成陶瓷芯初坯，然后对所述陶瓷芯初坯进行加热固化、浸渗和干燥，得到陶瓷芯坯体；所述干态粘接剂为可溶性盐；
(2)将步骤(1)得到的陶瓷芯坯体进行烧结，随炉冷却后即得到所述可溶性陶瓷芯。
2.根据权利要求1所述的制备方法，其特征在于，步骤(1)中，所述微滴喷射粘结成型工艺中的打印参数为：打印层高0.05mm～0.20mm，粘接剂饱和度80％～160％；所述加热固化的温度为180℃～210℃，时间为3h～6h。
3.根据权利要求1或2所述的制备方法，其特征在于，步骤(1)中，所述陶瓷粉骨料为石英、氧化铝、氧化锆、氧化钇中的一种或几种的混合物；所述干态粘结剂为氯化盐、硫酸盐、硅酸盐、磷酸盐、偏磷酸盐中的一种或几种的混合物；所述的陶瓷粉骨料和所述干态粘结剂的粒径为325目～1000目。
4.根据权利要求3所述的制备方法，其特征在于，所述的混合粉料中，所述干态粘结剂所占质量分数为15％～50％。
5.根据权利要求1-4任一项所述的制备方法，其特征在于，步骤(1)中，所述浸渗使用的浸渗液为醇基浸渗液，所述醇基浸渗液为纳米SiO2醇基分散液、纳米ZrO2醇基分散液或纳米TiO2醇基分散液中的至少一种，浸渗时间为30s～3min，浸渗方式为常压浸渗或者真空浸渗，真空浸渗时真空度为0～50KPa，质量分数为10％～40％；所述浸渗液用于渗透进陶瓷芯坯体的孔隙中，使其在烧结过程中可保持形状完整，避免坯体坍塌。
6.根据权利要求1所述的制备方法，其特征在于，步骤(2)中，所述烧结分为两个阶段，分别为在650℃～800℃下烧结1h～3h，然后在1100℃～1500℃下烧结1h～3h，烧结过程中升温速率为2～5℃/min。
7.一种利用权利要求1-6任一项所述方法制备得到的可溶性陶瓷芯。
8.如权利要求7所述的可溶性陶瓷芯在精密铸造中的应用。
9.根据权利要求8所述的应用，其特征在于，所述可溶性陶瓷芯与型壳相互配合，用于空腔结构件的精密铸造。
10.根据权利要求8或9所述的应用，其特征在于，将浇注完成后的构件放入水中，陶瓷芯遇水发生反应会开裂溃散，与结构件分离，形成空腔结构件。
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