CN110304926A - 一种氮化硅泥料及其制备方法和氮化硅陶瓷件 - Google Patents
一种氮化硅泥料及其制备方法和氮化硅陶瓷件 Download PDFInfo
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Abstract
本发明涉及3D打印技术领域,尤其涉及一种氮化硅泥料及其制备方法和氮化硅陶瓷件。本发明公开了一种氮化硅泥料,按重量份数计,由以下组分制成:氮化硅粉体100份;聚乙二醇1~5份;聚丙烯酸1~5份;聚乙烯醇0.5~3份;2‑氨基‑2‑甲基‑1‑丙醇0.5~3份;去离子水10~150份;氮化硅粉体包括氮化硅和Al2O3‑Re2O3,所述Al2O3‑Re2O3中的Re选自Sc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb或Lu。本发明中,氮化硅泥料组分简单,且固含量高,从而使得氮化硅泥料的制备时间缩短,稳定性提高,保存时间长。
Description
技术领域
本发明涉及3D打印技术领域,尤其涉及一种氮化硅泥料及其制备方法和氮化硅陶瓷件。
背景技术
3D打印技术是制造领域正在迅速发展的一项新兴技术,被称为“具有工业革命意义的制造技术”。Si3N4陶瓷由于具有综合机械性能高、耐高温、耐磨损、耐腐蚀等优点而作为重要的结构陶瓷材料,被广泛应用于航空航天、装备制造、能源化工、生物医疗等领域,但Si3N4陶瓷材料在较复杂结构的成型制造中仍具有较大的挑战,限制了其在各行各业的深入发展。因此将Si3N4陶瓷材料应用于3D打印技术成为该材料用于制造发展的必然趋势。
针对氮化硅陶瓷材料的3D打印,现有的氮化硅陶瓷材料制备中需要添加烧结助剂、树脂、分散剂和光引发剂等多种原料,添加原料过多,使得其制备过程复杂,导致制备得到的泥料稳定性差。
发明内容
本发明提供了一种氮化硅泥料及其制备方法和氮化硅陶瓷件,解决了现有的光固化氮化硅陶瓷泥料的原料繁多,导致其制备得到的泥料稳定性差的问题。
其具体技术方案如下:
本发明提供了一种氮化硅泥料,由以下组分制成:
氮化硅粉体100份;
聚乙二醇1~5份;
聚丙烯酸1~5份;
聚乙烯醇0.5~3份;
2-氨基-2-甲基-1-丙醇0.5~3份;
去离子水10~150份;
氮化硅粉体包括氮化硅和Al2O3-Re2O3;
所述Al2O3-Re2O3中的Re选自Sc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb或Lu,优选为Y、La、Gd、Yb或Lu,更优选为Y。
本发明中,Al2O3-Re2O3为烧结助剂;聚乙二醇为增塑分散剂,在氮化硅泥料中主要起到粘结和分散的作用;聚丙烯酸为分散剂,在氮化硅泥料中主要起到分散的作用;聚乙烯醇为粘合剂,在氮化硅泥料中主要起粘合的作用;2-氨基-2-甲基-1-丙醇用于调节氮化硅泥料的pH值,同时促进泥料湿润,保持水分和分散的作用。
本发明中,聚乙二醇分子量为1000~4000,优选为1800~2200,聚丙烯酸分子量为2000~5000,优选为3000,聚乙烯醇的分子量为110000~130000,优选为120000。
本发明中,氮化硅纯度>99.99%,粒径<10μm;Al2O3纯度为>99.99%,粒径<0.2μm;Re2O3纯度>99.99%;Al2O3-Re2O3的质量百分数比为1~99%:99~1%。
本发明中,氮化硅泥料组分简单,且固含量高,从而使得氮化硅泥料的制备时间缩短,稳定性提高,保存时间长。
优选地,按重量份数计,
所述氮化硅粉体100份;
所述聚乙二醇3份;
所述聚丙烯酸2份;
所述聚乙烯醇1份;
所述2-氨基-2-甲基-1-丙醇3份;
所述去离子水30-60份,更优选为45-50份。
优选地,按重量份数计,
所述氮化硅95~90份,更优选为90份;
所述Al2O3-Re2O3 5~10份,更优选为10份。
优选地,所述氮化硅泥料的湿度为25~50%,更优选为30%。
本发明还提供了上述氮化硅泥料的制备方法,包括以下步骤:
步骤1:将氮化硅与Al2O3-Re2O3混合并溶于第一有机溶剂中,进行球磨,除去所述第一有机溶剂后,得到氮化硅粉体;
步骤2:将所述氮化硅粉体与聚乙二醇、聚丙烯酸、聚乙烯醇和2-氨基-2-甲基-1-丙醇溶于第二有机溶剂中进行混合后,除去第二有机溶剂后,加入去离子水,得到氮化硅泥料。
本发明氮化硅泥料制备方法简单,大大缩短了氮化硅泥料的制备周期,适合工业化生产。
优选地,所述氮化硅的粒径为80~160目,更优选为100目。
优选地,步骤1所述球磨的速率为200~300rpm,时间为6-8h,更优选为250rpm,6h。
本发明步骤1中,所述第一有机溶剂为去离子水或无水乙醇;采用旋转蒸发除去第一有机溶剂。
本发明步骤2中,所述第二有机溶剂为去离子水或无水乙醇;
所述将所述氮化硅粉体与聚乙二醇、聚丙烯酸、聚乙烯醇和2-氨基-2-甲基-1-丙醇溶于第二有机溶剂中进行混合具体为:
分别将聚乙二醇、聚丙烯酸、聚乙烯醇溶于第二有机溶剂中,再分别进行搅拌,然后将所述氮化硅粉体依次与三份溶液进行混合,得到混合浆料;将2-氨基-2-甲基-1-丙醇加入混合浆料中,混合均匀;所述搅拌采用磁力搅拌,搅拌的速率为150~300rpm,时间为20min,温度为30~50℃。采用上述方法可以保证氮化硅各原料混合均匀。
优选地,步骤2所述混合得到的混合物的pH值为9~11,更优选为10。
优选地,步骤2所述球磨的速率为200~300rpm,时间为2~6h,更优选为200rpm,4h。
本发明还提供了一种氮化硅陶瓷件,由以下制备方法制得:
将上述氮化硅泥料进行3D打印,得到氮化硅陶瓷件;
所述3D打印为直写式成型3D打印技术。
从以上技术方案可以看出,本发明具有以下优点:
本发明提供了一种氮化硅泥料,该氮化硅泥料组分简单,添加剂非常少,且固含量高,从而使得氮化硅泥料的制备时间缩短,稳定性提高,保存时间长。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅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性的前提下,还可以根据这些附图获得其它的附图。
图1为本发明实施例3提供的氮化硅陶瓷件的实物图;
图2为本发明对比例1提供的氮化硅陶瓷件的实物图。
具体实施方式
本发明实施例提供了一种氮化硅泥料及其制备方法和氮化硅陶瓷件,用于解决现有的光固化氮化硅陶瓷泥料的原料繁多,导致其制备得到的泥料稳定性差的问题。
为使得本发明的发明目的、特征、优点能够更加的明显和易懂,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,下面所描述的实施例仅仅是本发明一部分实施例,而非全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其它实施例,都属于本发明保护的范围。
本发明提供的氮化硅泥料及其制备方法和氮化硅陶瓷件中所用的原料及试剂均可由市场购得。
以下就本发明所提供的一种氮化硅泥料及其制备方法和氮化硅陶瓷件做进一步说明。
实施例1
(1)以Si3N4为原料,以Al2O3-Y2O3为烧结助剂,按质量分数比Si3N4:Al2O3-Y2O3=90%:10%,即取90g Si3N4和10g Al2O3-Y2O3配料,以无水乙醇为溶剂,使用桨叶式搅拌装置将三者混合为均匀的Si3N4浆料;将此浆料利用滚式球磨机以250rpm的速度进行球磨6h,经旋转蒸发、过100目筛后得到含烧结助剂的氮化硅粉体;
(2)取三只烧杯均加入30g无水乙醇(酒精),分别加入3g的分子量为1800~2200的聚乙二醇(PEG)、2g分子量为3000的聚丙烯酸(PAA)和1g分子量为120000的聚乙烯醇(PVA),分别将烧杯置于磁力搅拌装置上以40℃、170rpm的转速搅拌20min直至各溶质完全溶于乙醇中;
(3)取步骤(2)所得的氮化硅粉体质量100g,将步骤(2)配置的三份溶液缓慢加入其中,在此过程中桨叶搅拌装置不停运行,直至得到均匀混合浆料;
(4)向步骤(3)的混合浆料中添加3g的2-氨基-2-甲基-1-丙醇(AMP),混合均匀,调节其PH为10,并将该浆料倒入球磨罐中,加入200g的Si3N4磨球;
(5)将步骤(4)的浆料利用滚式球磨机以200rpm的速度进行球磨4h,取出后静置5分钟;经旋转蒸发、过100目筛后得到有聚乙二醇、聚丙烯酸、聚乙烯醇和2-氨基-2-甲基-1-丙醇均匀涂覆的氮化硅颗粒。
(6)取100g步骤(5)得到的氮化硅颗粒,缓慢添加43g去离子水,得到湿度为30%的氮化硅泥料。
实施例2
(1)以Si3N4为原料,以Al2O3-Y2O3为烧结助剂,按质量分数比Si3N4:Al2O3-Y2O3=90%:10%,即取90g Si3N4和10g Al2O3-Y2O3配料,以无水乙醇为溶剂,使用桨叶式搅拌装置将三者混合为均匀的Si3N4浆料;将此浆料利用滚式球磨机以250rpm的速度进行球磨6h,经旋转蒸发、过100目筛后得到含烧结助剂的氮化硅粉体;
(2)取三只烧杯均加入30g无水乙醇(酒精),分别加入3g的分别加入3g的分子量为1800~2200的聚乙二醇(PEG)、2g分子量为3000的聚丙烯酸(PAA)和1g分子量为120000的聚乙烯醇(PVA),分别将烧杯置于磁力搅拌装置上以40℃、170rpm的转速搅拌20min直至各溶质完全溶于乙醇中;
(3)取步骤(2)所得的氮化硅粉体质量100g,将步骤(2)配置的三份溶液缓慢加入其中,在此过程中桨叶搅拌装置不停运行,直至得到均匀混合浆料;
(4)向步骤(3)的浆料中添加3g 2-氨基-2-甲基-1-丙醇(AMP),混合均匀,调节其PH为10,并将该浆料倒入球磨罐中,加入200g的Si3N4磨球;
(5)将步骤(4)的浆料利用滚式球磨机以200rpm的速度进行球磨4h,取出后静置5分钟;经旋转蒸发、过100目筛后得到有聚乙二醇、聚丙烯酸、聚乙烯醇和2-氨基-2-甲基-1-丙醇均匀涂覆的氮化硅颗粒。
(6)取100g步骤(5)得到的氮化硅颗粒,缓慢添加54g去离子水,得到湿度为35%的氮化硅泥料。
对比例1
(1)以Si3N4为原料,以Al2O3-Y2O3为烧结助剂,按质量分数比Si3N4:Al2O3-Y2O3=90%:10%,即取90g Si3N4和10g Al2O3-Y2O3配料,以无水乙醇为溶剂,使用桨叶式搅拌装置将三者混合为均匀的Si3N4浆料;将此浆料利用滚式球磨机以250rpm的速度进行球磨6h,经旋转蒸发、过100目筛后得到含烧结助剂的氮化硅粉体;
(2)取三只烧杯均加入30g无水乙醇(酒精),分别加入3g的分子量为1800~2200的聚乙二醇(PEG)、2g分子量为3000的聚丙烯酸(PAA)和1g分子量为120000的聚乙烯醇(PVA),分别将烧杯置于磁力搅拌装置上以40℃、170rpm的转速搅拌20min直至各溶质完全溶于乙醇中;
(3)取步骤(2)所得的氮化硅粉体质量100g,将步骤(2)配置的三份溶液缓慢加入其中,在此过程中桨叶搅拌装置不停运行,直至得到均匀混合浆料;
(4)将步骤(3)的浆料倒入球磨罐中,加入200g的Si3N4磨球;用滚式球磨机以200rpm的速度进行球磨4h,取出后静置5分钟;经旋转蒸发、过100目筛后得到有聚乙二醇、聚丙烯酸和聚乙烯醇等均匀涂覆的氮化硅颗粒。
(5)取100g步骤(4)得到的氮化硅颗粒,缓慢添加54g去离子水,得到湿度为35%的氮化硅泥料。
实施例3
将实施例2和对比例1制备得到的氮化硅泥料采用直写式成型技术(Robocastingor Direct Ink Writing),得到氮化硅陶瓷件。
如图1所示,本实施例氮化硅陶瓷件,其泥料流动性、成型性、均匀性等均表现良好,经打印喷头挤出后,可以根据预先设计的结构,稳定成型,且稳定性好。
如图2所示,对比例1与实施例2氮化硅泥料相同喷头挤出的泥料成型性能差,虽然具有良好的流动性,但是挤出后随即塌陷,层与层间界限完全混淆,因此无法3D成型。
以上所述,以上实施例仅用以说明本发明的技术方案,而非对其限制;尽管参照前述实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。
Claims (10)
1.一种氮化硅泥料,其特征在于,按重量份数计,由以下组分制成:
氮化硅粉体100份;
聚乙二醇1~5份;
聚丙烯酸1~5份;
聚乙烯醇0.5~3份;
2-氨基-2-甲基-1-丙醇0.5~3份;
去离子水10~150份;
氮化硅粉体包括氮化硅和Al2O3-Re2O3;
所述Al2O3-Re2O3中的Re选自Sc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb或Lu。
2.根据权利要求1所述的氮化硅泥料,其特征在于,按重量份数计,
所述氮化硅粉体100份;
所述聚乙二醇3份;
所述聚丙烯酸2份;
所述聚乙烯醇1份;
所述2-氨基-2-甲基-1-丙醇3份;
所述去离子水30-60份。
3.根据权利要求1所述的氮化硅泥料,其特征在于,按质量百分数计,
所述氮化硅95~90份;
所述Al2O3-Re2O3 5~10份。
4.根据权利要求1所述的氮化硅泥料,其特征在于,所述氮化硅泥料的湿度为25~50%。
5.权利要求1至4任意一项所述的氮化硅泥料的制备方法,其特征在于,包括以下步骤:
步骤1:将氮化硅与Al2O3-Re2O3混合并溶于第一有机溶剂中,进行球磨,除去所述第一有机溶剂后,得到氮化硅粉体;
步骤2:将所述氮化硅粉体与聚乙二醇、聚丙烯酸、聚乙烯醇和2-氨基-2-甲基-1-丙醇溶于第二有机溶剂中进行混合,进行球磨,除去第二有机溶剂后,加入去离子水,得到氮化硅泥料。
6.根据权利要求5所述的制备方法,其特征在于,步骤2所述混合得到的混合物的pH值为9~11。
7.根据权利要求5所述的制备方法,其特征在于,步骤1所述球磨的速率为200~300rpm,时间为6-8h。
8.根据权利要求5所述的制备方法,其特征在于,步骤2所述球磨的速率为200~300rpm,时间为2~6h。
9.根据权利要求5所述的制备方法,其特征在于,所述氮化硅的粒径为80~160目。
10.一种氮化硅陶瓷件,其特征在于,由以下制备方法制得:
将权利要求1至4任意一项所述的氮化硅泥料进行3D打印,得到氮化硅陶瓷件;
所述3D打印为直写式成型3D打印技术。
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