CN106631038B - 一种喷嘴用高耐磨Si3N4基金刚石复合陶瓷材料及其制备方法 - Google Patents
一种喷嘴用高耐磨Si3N4基金刚石复合陶瓷材料及其制备方法 Download PDFInfo
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Abstract
本发明提出了一种喷嘴用高耐磨Si3N4基金刚石复合陶瓷材料,解决了现有技术中材料硬度低,耐磨性差,无法满足喷嘴对材料的高耐磨性需求;同时,还提出了喷嘴用高耐磨Si3N4基金刚石复合陶瓷材料的制备方法,解决了现有技术中陶瓷‑金刚石复合材料的制备对设备要求高,制备成本高,工艺复杂的问题。本发明提出的喷嘴用高耐磨Si3N4基金刚石复合陶瓷材料的制备方法获得高耐磨Si3N4基的金刚石复合陶瓷材料,相对密度高,硬度为20~40GPa,制备成本低,工艺简便且稳定。
Description
技术领域
本发明涉及陶瓷材料领域,尤其涉及喷嘴用高耐磨Si3N4基金刚石复合陶瓷材料和该材料的制备方法。
背景技术
喷嘴广泛应用于工业领域,是表面清洗、强化和喷射切割等设备的关键部件之一,属于易磨耗部件。目前,国内外常用的喷嘴材料主要为金属、硬质合金等,此类材料的硬度低、耐磨性差,导致喷嘴使用寿命短,频繁更换不仅增加成本,降低生产率,而且增大了工人的劳动强度。陶瓷材料因具有硬度高、耐磨损等优点,是喷嘴的理想材料之一,陶瓷喷嘴一直是我国喷嘴技术研发的重点。金刚石因具有极高的硬度,是制造喷嘴的理想材料,陶瓷基的金刚石复合材料可进一步改善陶瓷材料的硬度,增加材料的耐磨性,但金刚石复合材料烧结困难,高温下易发生氧化与石墨化,是材料制备的一大技术难题。为降低或避免金刚石的氧化与石墨化,通常采用放电等离子烧结、高温高压烧结、化学气相沉积的方法制备材料,对设备要求高,制备成本高且工艺复杂,不易控制。例如,Huang等采用放电等离子烧结方法制备Si3N4基的金刚石陶瓷材料,整个实验过程中脉冲电流的脉宽为10ms,间隔时间为5ms,最大压力达到 100MPa,升温速率为200℃/min,对减小或避免金刚石的石墨化起到了显著作用(Shuigen Huang,Akhilesh Kumar Swarnakar,Kim Vanmeensel,Jef Vleugels.Diamond dispersed Si3N4 composites obtained by pulsed electric currentsintering. Journal of the European Ceramic Society,2013,33(6):1237–1247)。
发明内容
本发明提出的一种喷嘴用高耐磨Si3N4基金刚石复合陶瓷材料,解决了现有技术中材料硬度低,耐磨性差,无法满足喷嘴对材料的高耐磨性需求;同时,还提出了喷嘴用高耐磨Si3N4基金刚石复合陶瓷材料的制备方法,解决了现有技术中陶瓷-金刚石复合材料的制备对设备要求高,制备成本高,工艺复杂的问题。
为了实现上述技术方案,本发明提供一种喷嘴用高耐磨Si3N4基金刚石复合陶瓷材料,按质量分数比包括95~90%Si3N4,5~10%Al2O3-Re2O,10~30%镀M 的金刚石,其中,Re为Sc,Y,La,Ce,Pr,Nd,Pm,Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb, Lu中之任一或任意组合;M为Ni,Ti,Cu中之任一或任意组合;所述复合陶瓷材料相对密度高,硬度为20~40GPa。
还提出了一种喷嘴用高耐磨Si3N4基金刚石复合陶瓷材料的制备方法,单位为质量分数比,
步骤1,Si3N4浆料的制备
以Si3N4粉体为原料,以Al2O3-Re2O3为烧结助剂,按质量分数比Si3N4: Al2O3-Re2O3=95~90%:5~10%配料,以乙醇为溶剂,其中,以Si3N4球为球磨介质,球料质量比为2~5:1,在行星球磨机上混合8~12h,得到Si3N4浆料;
步骤2,Si3N4-金刚石浆料的制备
将质量分数10~30%镀M的金刚石微粉添加进步骤1制备的Si3N4浆料中,经搅拌器按200~400r/min转速搅拌混合浆料15~30min,得到混合均匀的Si3N4- 金刚石浆料;
步骤3,Si3N4-金刚石复合材料的制备
将步骤2所得混合浆料经干燥、过100目筛造粒,经30MPa压力热压烧结, 冷却后得到高耐磨的Si3N4基金刚石复合材料;
得到的高耐磨Si3N4基的金刚石复合陶瓷材料,相对密度大于98%,硬度为 20~40GPa。
步骤1中,Al2O3-Re2O3中,Re为Sc,Y,La,Ce,Pr,Nd,Pm,Sm,Eu,Gd,Tb,Dy, Ho,Er,Tm,Yb,Lu中的任一或任意组合。
步骤1中,Si3N4粉纯度为95~100%,粒径<10μm。
步骤1中,Al2O3纯度为>99.99%,粒径<0.1μm;Re2O3纯度99.9%;所述 Al2O3-Re2O3的质量分数比为1~99%:99~1%。
步骤2中,M为Ni,Ti,Cu中的任一或任意组合。
步骤2中,所用镀M金刚石微粉的粒径为10~30μm。
步骤3中,热压烧结的升温速率为10~15℃/min,烧结温度1600~1750℃,升温保温时间30~60min,保护气氛为N2或Ar。
获得高耐磨Si3N4基的金刚石复合陶瓷材料,相对密度高,硬度为20~40GPa,制备成本低,工艺简便且稳定。
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他的附图。
图1为喷嘴用高耐磨Si3N4基金刚石复合陶瓷材料的XRD检测图。
图2为喷嘴用高耐磨Si3N4基金刚石复合陶瓷材料表面显微照片。
具体实施方式
下面将结合本发明实施例中的附图,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。
实施例一:
(1)以Si3N4粉体为基体原料,以Al2O3-Y2O3为烧结助剂,按质量分数比 Si3N4:Al2O3-Y2O3=90%:10%配料,其中Al2O3-Y2O3的质量分数比为4%:5%,以乙醇为溶剂,以Si3N4球为球磨介质,球料比为3:1,在行星球磨机上混合8h,得到Si3N4浆料。
(2)将质量分数30%的金刚石微粉(镀Ti,粒径10μm)添加进Si3N4浆料,经搅拌器以250r/min转速搅拌混合浆料20min后,得到混合均匀的Si3N4-金刚石浆料。
(3)将Si3N4-金刚石混合浆料经干燥、造粒(过100目筛),经热压烧结,压力30MPa,升温速率为10℃/min,烧结温度1600℃,保温时间为45min,保护气氛为N2,冷却后得到高耐磨的氮化硅/金刚石复合材料。
制备得到的高耐磨Si3N4基的金刚石复合陶瓷材料,相对密度为98%,硬度为34GPa。
实施例二:
(1)以Si3N4粉体为基体原料,以Al2O3-Lu2O3为烧结助剂,按质量分数比 Si3N4:Al2O3-Y2O3=95%:5%配料,其中Al2O3-Lu2O3的质量分数比为3%:2%,以乙醇为溶剂,以Si3N4球为球磨介质,球料比为3:1,在行星球磨机上混合10h,得到Si3N4浆料。
(2)将质量分数20%的金刚石微粉(镀Cu,粒径20μm)添加进Si3N4浆料,经搅拌器以300r/min转速搅拌混合浆料25min后,得到混合均匀的Si3N4- 金刚石浆料。
(3)将Si3N4-金刚石混合浆料经干燥、造粒(过100目筛),经热压烧结,压力30MPa,升温速率为15℃/min,烧结温度1650℃,保温时间为50min,保护气氛为Ar,冷却后得到高耐磨的氮化硅/金刚石复合材料。
制备得到的高耐磨Si3N4基的金刚石复合陶瓷材料,相对密度为99%,硬度为27GPa。
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、改进等,均应包含在本发明的保护范围之内。
Claims (4)
1.一种喷嘴用高耐磨Si3N4基金刚石复合陶瓷材料的制备方法,其特征在于:
所述的材料包括以下组分,其中,单位为质量分数比:
Si3N4 95~90%,
Al2O3-Re2O3 5~10%,
镀M的金刚石10~30%,
上述组分的总质量分数为100%;
其中,Re为Sc,Y,La,Ce,Pr,Nd,Pm,Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb,Lu中之任一或任意
组合;M为Ni,Ti,Cu中之任一或任意组合;
包括以下步骤:
步骤1,Si3N4浆料的制备
以Si3N4粉体为原料,以Al2O3-Re2O3为烧结助剂,按质量分数比Si3N4:Al2O3-Re2O3=95~90%:5~10%配料,以无水乙醇为溶剂,其中,以Si3N4球为球磨介质,球料质量比为2~5:1,
在行星球磨机上混合8~12h,得到Si3N4浆料;
步骤2,Si3N4-金刚石浆料的制备
将质量分数10~30%镀M的金刚石微粉添加进步骤1制备的Si3N4浆料中,经搅拌器按200~400r/min转速搅拌混合浆料15-30min,得到混合均匀的Si3N4-金刚石浆料;
步骤3,Si3N4-金刚石复合材料的制备
将步骤2所得混合浆料经干燥、过100目筛造粒,经30MPa压力热压烧结,冷却后得到高耐磨的Si3N4基金刚石复合材料;
其中,热压烧结的升温速率为10~15℃/min,烧结温度1600~1750℃,升温保温时间30~60min,保护气氛为N2或Ar;
得到的高耐磨Si3N4基的金刚石复合陶瓷材料,相对密度高,硬度为20~40GPa。
2.根据权利要求1所述的Si3N4基金刚石复合陶瓷材料的制备方法,其特征在于:步骤1中,Si3N4粉纯度为95~100%,粒径<10μm。
3.根据权利要求1所述的Si3N4基金刚石复合陶瓷材料的制备方法,其特征在于:步骤1中,Al2O3纯度为>99.99%,粒径<0.1μm;Re2O3纯度99.9%;所述Al2O3-Re2O3的质量分数比为1~99%:99~1%。
4.根据权利要求1所述的Si3N4基金刚石复合陶瓷材料的制备方法,其特征在于:步骤2中,所用镀M金刚石微粉的粒径为10~30μm。
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