CN112171848A - 一种光固化碳化硅陶瓷浆料及其制备方法与应用 - Google Patents

一种光固化碳化硅陶瓷浆料及其制备方法与应用 Download PDF

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CN112171848A
CN112171848A CN202011051644.5A CN202011051644A CN112171848A CN 112171848 A CN112171848 A CN 112171848A CN 202011051644 A CN202011051644 A CN 202011051644A CN 112171848 A CN112171848 A CN 112171848A
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silicon carbide
carbide ceramic
photocuring
ceramic slurry
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刘耀
江泽星
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Jiangxi Jinshi 3d Intelligent Manufacturing Technology Co ltd
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Abstract

本发明提供了一种光固化碳化硅陶瓷浆料及其制备方法与应用，属于功能陶瓷领域。本发明提供的碳化硅陶瓷浆料由改性丙烯酸酯、碳化硅粉末、稀释剂、表面改性剂、分散剂、光引发剂按照质量比20‑40:10‑70:10‑30:1‑10:1‑10:1‑6混合制得；稀释剂为1，6‑已二醇双丙烯酸酯、丙烯酸羟乙酯、三羟甲基丙烷三丙烯酸酯中的一种或者几种任意比例的混合；表面改性剂为KH550和KH570中的一种或者几种任意比例的混合；分散剂为KOS110和KOS190中的一种或者几种；光引发剂为TPO。

Description

一种光固化碳化硅陶瓷浆料及其制备方法与应用
技术领域
本发明涉及功能陶瓷领域，尤其涉及一种光固化碳化硅陶瓷浆料及其制备方法与应用。
背景技术
SiC陶瓷不仅具有优良的常温力学性能，如高的抗弯强度、优良的抗氧化性、良好的耐腐蚀性、高的抗磨损以及低的摩擦系数，而且高温力学性能(强度、抗蠕变性等)是已知陶瓷材料中最佳的。但是在高致密、高硬度的形状复杂陶瓷异形件，由于陶瓷本身的脆性，加上制备的复杂模具增加了生产成本和周期，制约了它的发展。
增材制造技术将传统的“去除”和“等体积”制造变化为“增加”制造，具有开发周期短、不需模具、成本低等许多优势。它是基于分层-叠加原理，首先在三维造型软件中生成零件的三维模型，然后对其进行切片处理，把每层的信息输入到制造装备，通过材料的逐层堆积获得最终任意复杂的三维实体零件。其中，光固化技术以制备复杂、致密的陶瓷而成为研究热点。SLA技术是以光敏树脂为原料，紫外光源根据三维模型的截面信息对液态光敏树脂进行扫描，实现单层固化。然后，工作台下降一个层厚的高度，进而得到陶瓷零件。由于SLA技术具有制造精度高(±0.1mm)、表面质量好、能够制造精细零件的优点，它已成功应用于医学与生物领域(如牙齿和骨骼修复)、微技术领域(如传感器、压电元件及光子晶体)及机械耐热结构领域(如涡轮叶片)等。
然而，目前国内外在高精度碳化硅SLA成型技术方面的研究刚刚起步，尽管光固化已经成形出复杂、致密的氧化物陶瓷。而对于非氧化物陶瓷还没有展开系统的研究。尤其是碳化硅陶瓷目前还没有展开系统的研究，陶瓷浆料的难以成型，严重制约了高密度、高性能的复杂型陶瓷零件的成型。本发明提供的高精度光固化碳化硅结构陶瓷成型和烧结的制备方法。
本发明通过成份的调控，成形出了复杂、结构的碳化硅陶瓷，解决了陶瓷本身收缩率大、致密度低的问题。得到的高精度、高性能的陶瓷产品，使其能够更好地应用于航天事业、医疗和工业领域。
发明内容
针对上述问题，本发明的目的在于通过调控各组份的成分，制备出了一有鉴于此，本发明的目的在于提供一种光固化碳化硅陶瓷浆料及其制备方法与应用，本发明提供的光固化碳化硅陶瓷浆料性能稳定，在光固化成型时，成型过程稳定，得到的碳化硅陶瓷性能稳定。
为了实现上述发明目的，本发明提供以下技术方案：
本发明提供了一种光固化碳化硅陶瓷陶瓷浆料，包括以下重量份数的组分：改性丙烯酸酯(WUA)、碳化硅粉末、稀释剂、分散剂、光引发剂按照质量比20-40:10-70:10-30:1-10:1-6混合制得。
优选地，所述碳化硅粉末的粒径为100-800nm。
优选地，稀释剂为1，6-已二醇双丙烯酸酯(HDDA)、丙烯酸羟乙酯(HEA)、三羟甲基丙烷三丙烯酸酯(TMPTA)中的一种或者几种任意比例的混合。
优选地，分散剂为KOS110和KOS190中的一种或者几种任意比例的混合。
优选地，所述光引发剂为TPO组成。
在本发明中，所述碳化硅陶瓷粉末的粒径优选为100-800nm，更优选为400-600nm。本发明对所述碳化硅粉末的来源没有任何特殊的限定，采用本领域技术人员熟知的市售商品即可。
本发明还提供了上述技术方案所述光固化碳化硅陶瓷浆料的制备方法，包括以下步骤：
(1)将碳化硅陶瓷粉末与分散剂按照10-70:1-6的比例进行搅拌球磨；再进行干燥，最终得到改性后的碳化硅粉体；
(2)将改性丙烯酸酯、稀释剂和光引发剂按照质量比20-40:10-30:1-6的比例进行搅拌球磨，得到树脂体系；
(3)将所述步骤(2)得到的碳化硅陶瓷粉末与所述步骤(1)得到的树脂体系混合，得到光固化碳化硅陶瓷浆料；
对所述步骤(1)和(2)没有顺序限定。
本发明将碳化硅粉末和分散剂依次经混合和干燥，得到碳化硅陶瓷粉末。本发明对所述混合的方式没有特殊的限定，采用本领域技术人员熟知的混合方式即可，具体的，如搅拌。搅拌速率为350-450r/min。所述搅拌的时间优选为5～20min，更优选为8～15min，最优选为10～12min。在本发明中，所述混合能够使碳化硅陶瓷粉体和分散剂充分混合。
在本发明中，所述干燥的温度优选为30～80℃，更优选为40～70℃，最优选为50～60℃。在本发明中，所述干燥的时间优选为24～48h，更优选为30～40h，最优选为34～36h。
本发明将活性稀释剂和光引发剂混合，得到树脂体系。本发明对所述混合的方式没有特殊的限定，采用本领域技术人员熟知的混合方式即可，具体的，如搅拌。在本发明中，所述搅拌的速率优选为350～450r/min，更优选为375～425r/min，最优选为400r/min。在本发明中，所述搅拌的时间优选为15～60min，更优选为20～50min，最优选为30～40min。
得到碳化硅陶瓷粉末和树脂体系后，本发明将所述碳化硅粉末与树脂体系混合，得到光固化碳化硅陶瓷浆料。本发明对所述混合的方式没有特殊的限定，采用本领域技术人员熟知混合方式即可，具体的，如搅拌。在本发明中，所述搅拌的速率优选为350～450r/min，更优选为375～425r/min，最优选为400r/min。在本发明中，所述搅拌的时间优选为30～60min，更优选为35～55min，最优选为40～50min。
本发明还提供了上述技术方案所述的光固化氮化硅陶瓷浆料在制备碳化硅陶瓷零件中的应用。
优选地，所述应用包括以下步骤：
(1)将光固化碳化硅陶瓷浆料进行光固化，形成坯体；
(2)对所述步骤(1)得到的坯体依次进行脱脂和烧结，得到碳化硅陶瓷零件。
本发明将光固化碳化硅陶瓷浆料进行光固化，形成坯体。在本发明中，所述光固化用光源的波长优选为365～450nm，更优选为380～420nm，最优选为390～410nm。本发明对所述光固化碳化硅浆料的光固化次数没有限定，本领域技术人员根据需要进行调整即可。在本发明中，每次光固化的时间优选4～10s，更优选5～9s，更优选6～8s。在本发明中，每次光固化后光固化产物的厚度优选为0.02～0.05mm，更优选0.03～0.04mm，最优选0.035mm。本发明优选对光固化碳化硅陶瓷浆料进行多次固化，提高光固化浆料的光固化效果，而且也能够制备出形状较复杂的坯体。
在本发明中，所述光固化优选在光固化设备中，按照预先设计的图形，得到坯体。本发明对图形没有特殊的限定，本领域技术人员根据需要进行设计即可。
得到坯体后，本发明将坯体依次进行脱脂和烧结，得到碳化硅陶瓷零件。在本发明中，所述脱脂的温度优选为500～800℃，更优选600～700℃，最优选650～700℃，脱脂的时间为60-120min，更优选为60-90min，最优选为80min。本发明中，所述升温至脱脂温度的升温速率优选为0.5～2℃/min，更优选为0.8～1.6℃/min，最优选为1.0～1.4℃/min。在本发明中，所述脱脂能够脱除坯体中的活性稀释剂。
在本发明中，所述烧结的压力优选为0.2～0.5MPa，更优选为0.3～0.4MPa，最优选为0.35MPa。在本发明中，所述烧结的温度优选为1100～1250℃，更优选为1150～1250℃，最优选为1200～1250℃，所述烧结的时间优选为48-96h，更优选为72-96h，最优选为80h。本发明中，所述烧结能够使碳化硅零件。
本发明的有益效果：
本发明提供的光固化碳化硅浆料性能稳定，均匀性和分散性好。
采用本发明的方法制备的碳化硅陶瓷零件力学性能稳定，且制备方法简单，耗时短，成本低。。
具体实施方式
为了更清楚、完整的描述本发明的技术方案，以下通过具体实施例进一步详细说明本发明，应当理解，此处所描述的具体实施例仅用于解释本发明，并不用于限定本发明，可以在本发明权利限定的范围内进行各种改变。
实施例1-3和对比例1-3
一种光固化碳化硅陶瓷陶瓷浆料，包括以下组分：碳化硅粉末、丙烯酸酯、稀释剂、分散剂、光引发剂按照质量比混合制得。配方(质量比)如表1所示：
表1
Figure BDA0002709740850000051
光固化碳化硅浆料的制备方法，包括以下步骤：
(1)将碳化硅粉末与分散剂进行搅拌球磨；其次再进行干燥，干燥，最终得到分散好的碳化硅粉体；
(2)将丙烯酸酯、稀释剂和光引发剂搅拌球磨，得到树脂体系；
(3)将所述步骤(2)得到的碳化硅陶瓷粉末与所述步骤(1)得到的树脂体系混合，得到光固化碳化硅陶瓷浆料。
各步骤参数见表2所示。
表2
Figure BDA0002709740850000061
光固化碳化硅浆料在制备碳化硅陶瓷的应用，包括以下步骤；
(1)将光固化碳化硅料进行光固化，形成坯体；
(2)对得到的坯体依次进行脱脂和烧结，得到碳化硅陶瓷零件。
其中，光固化、脱脂、烧结的具体参数见表3所示。
表3
Figure BDA0002709740850000071
采用力学性能测试标准，测试上述实施例和对比例制备的碳化硅陶瓷，碳化硅陶瓷具有很好的力学性能。测试结果如表4所示。
表4
Figure BDA0002709740850000072
Figure BDA0002709740850000081
最后需要强调的是，以上所述仅为本发明的优选实施例，并不用于限制本发明，对于本领域的技术人员来说，本发明可以有各种变化和更改，凡在本发明的精神和原则之内，所做的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (9)

1.一种光固化碳化硅陶瓷浆料，其特征在于，由改性丙烯酸酯、碳化硅粉末、稀释剂、分散剂、光引发剂按照质量比20-40:10-70:10-30:1-10:1-6混合制得。
2.根据权利要求1所述的一种光固化碳化硅陶瓷浆料，其特征在于，所述的稀释剂为1，6-已二醇双丙烯酸酯、丙烯酸羟乙酯、三羟甲基丙烷三丙烯酸酯中的一种或者几种任意比例的混合。
3.根据权利要求1所述的一种光固化碳化硅陶瓷浆料，其特征在于，所述的分散剂为KOS110、和KOS190中的一种或者几种任意比例的混合。
4.根据权利要求1所述的一种光固化碳化硅陶瓷浆料，其特征在于，所述碳化硅粉末的粒径为100-800nm。
5.根据权利要求1所述的光固化碳化硅陶瓷浆料，其特征在于，所述光引发剂为TPO。
6.权利要求1～5任一项所述光固化碳化硅陶瓷浆料的制备方法，其特征在于，包括以下步骤：
(1)将改性丙烯酸酯、稀释剂和光引发剂按照质量比20-40:10-30:1-6的比例进行搅拌球磨，得到树脂体系；
(2)将碳化硅陶瓷粉末与分散剂按照10-70:1-6的比例进行搅拌球磨，其次再进行干燥，最终得到分散好的碳化硅粉体。
(3)将所述步骤(2)得到的碳化硅陶瓷粉末与所述步骤(1)得到的树脂体系混合，得到光固化碳化硅陶瓷浆料。
7.权利要求1～5任一项所述的光固化碳化硅陶瓷浆料在制备碳化硅陶瓷零件中的应用。
8.根据权利要求7所述的应用，其特征在于，包括以下步骤：
(1)将光固化碳化硅陶瓷浆料进行光固化，形成高固相、低粘度的陶瓷浆料；
(2)对所述步骤(1)得到的坯体依次进行脱脂和烧结，得到碳化硅零件。
9.根据权利要求8所述的应用，其特征在于，所述步骤(1)中光固化用光源的波长为365～460nm。
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