CN107827464B - 一种燃烧合成制备ZrTiCB四元陶瓷粉体的方法 - Google Patents
一种燃烧合成制备ZrTiCB四元陶瓷粉体的方法 Download PDFInfo
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Abstract
本发明公开了一种燃烧合成制备ZrTiCB四元陶瓷粉体的方法,包括如下步骤:将锆粉、钛粉、碳粉和硼粉混匀并压坯,得到相对密度为40%~60%的预制块;采用通电钨丝发热诱导预制块中各原料组分之间发生自蔓延燃烧反应;反应得到的产物冷却后研磨制得Zr0.8Ti0.2C1‑xBx陶瓷粉体;其中,x取值范围为:0≤x≤0.15。本发明的燃烧合成制备Zr0.8Ti0.2C1‑xBx陶瓷的方法,使用单质粉末作为原料,利用原料间反应放热来完成材料的合成,具有工艺简单、制备周期短、能耗低成本低等特点。
Description
技术领域
本发明涉及燃烧合成技术领域。更具体地,涉及一种燃烧合成制备ZrTiCB四元陶瓷粉体的方法。
背景技术
ZrC、ZrB2均为常见的超高温陶瓷材料,具有高熔点、高硬度、高热导、抗热震、抗氧化、以及耐烧蚀等特性,可作为高温结构材料应用于高超声速飞行器的鼻锥、前缘以及超燃冲压发动机燃烧室的关键热端部件。Zr和Ti,C和B的原子半径接近,能够形成置换固溶体,使材料性能得到进一步的提升。已有报道,发现四元Zr0.8Ti0.2C0.74B0.26陶瓷具有优良的高温耐氧化、抗烧蚀等性能。通过Ti、B的固溶形成的四元Zr0.8Ti0.2C1-xBx陶瓷在硬度、韧性等机械性能,较ZrC、ZrB2等超高温陶瓷材料性能显著提升,是一类性能优异的新型超高温陶瓷材料。
目前Zr0.8Ti0.2C1-xBx体系的制备方法包括反应熔渗、包埋渗,然而现有的方法制备周期长,工艺复杂,成本高,且产物中的B含量不易调控,无法获得Zr、Ti、C、B比例稳定的产物。
因此,本发明提供了一种B含量可控的燃烧合成制备ZrTiCB四元陶瓷粉体的方法。
发明内容
本发明的一个目的在于提供一种燃烧合成制备ZrTiCB四元陶瓷粉体的方法。
为达到上述目的,本发明采用下述技术方案:
一种燃烧合成制备ZrTiCB四元陶瓷粉体的方法,包括如下步骤:
将锆粉、钛粉、碳粉和硼粉混匀并压坯,得到相对密度为40%~60%的预制块;采用通电钨丝发热诱导预制块中各原料组分之间发生自蔓延燃烧反应;反应得到的产物冷却后研磨制得Zr0.8Ti0.2C1-xBx陶瓷粉体;其中,x取值范围为:0≤x≤0.15。本发明采用的燃烧合成法是一种利用原料自身反应放热完成材料合成的制备方法,具有工艺简单、制备周期短、低能耗低成本等优势;此外,通过Zr、Ti、C、B原料比例的精确控制,同时利用粉体原料之间的强放热反应,可燃烧合成制得四元Zr0.8Ti0.2C1-xBx陶瓷。
优选地,所述锆粉、钛粉、碳粉和硼粉的摩尔比为0.8:0.2:1-x:x,其中0≤x≤0.15。
优选地,所述自蔓延燃烧反应在氩气气氛且气压为0.1~10MPa条件下进行。本发明中的气压范围内,气压的变化对陶瓷粉体的性能几乎无影响。
如无特殊说明,本发明所记载的任何范围包括端值以及端值之间的任何数值以及端值或者端值之间的任意数值所构成的任意子范围。
本发明的有益效果如下:
本发明的燃烧合成制备Zr0.8Ti0.2C1-xBx陶瓷的方法,使用单质粉末作为原料,利用原料间反应放热来完成材料的合成,具有工艺简单、制备周期短、能耗低成本低等特点。
附图说明
下面结合附图对本发明的具体实施方式作进一步详细的说明。
图1示出本发明中实施例1~4制得的Zr0.8Ti0.2C1-xBx陶瓷粉体的XRD图谱示意图;其中,(a)示出本发明实施例1制得的Zr0.8Ti0.2C陶瓷粉体的XRD图,(b)示出本发明实施例2制得的Zr0.8Ti0.2C0.95B0.05陶瓷粉体的XRD图,(c)示出本发明实施例3制得的Zr0.8Ti0.2C0.9B0.1陶瓷粉体的XRD图,(d)示出本发明实施例4制得的Zr0.8Ti0.2C0.85B0.15陶瓷粉体的XRD图。
具体实施方式
为了更清楚地说明本发明,下面结合优选实施例和附图对本发明做进一步的说明。本领域技术人员应当理解,下面所具体描述的内容是说明性的而非限制性的,不应以此限制本发明的保护范围。
本发明中,制备方法如无特殊说明则均为常规方法。所用的原料如无特别说明均可从公开的商业途径获得,所述百分比如无特殊说明均为质量百分比。
实施例1
一种陶瓷粉体的制备,包括如下步骤:
将Zr、Ti、C、B原料粉末按Zr:Ti:C:B=0.8:0.2:1:0的比例混合均匀并压坯,得到相对密度为40%的预制块;将预制块放入石墨模具中,并将整体置于反应釜中;然后在氩气作为保护气氛,气压为0.1MPa的反应釜中,利用通电钨螺旋丝发热诱导预制块中各原料之间发生自蔓延燃烧反应;反应的产物冷却后经破碎研磨,得到Zr0.8Ti0.2C陶瓷粉体。
对得到的粉末进行XRD测试,结果如图1(a)所示,结果表明,产物成分为Zr0.8Ti0.2C,无杂相生成。
实施例2
一种陶瓷粉体的制备,包括如下步骤:
将Zr、Ti、C、B原料粉末按Zr:Ti:C:B=0.8:0.2:0.95:0.05的比例混合均匀并压坯,得到相对密度为50%的预制块;将预制块放入石墨模具中,并将整体置于反应釜中;然后在氩气作为保护气氛,气压为0.1MPa的反应釜中,利用通电钨螺旋丝发热诱导预制块中各原料之间发生自蔓延燃烧反应;反应的产物冷却后经破碎研磨,得到Zr0.8Ti0.2C0.95B0.05陶瓷粉体。
对得到的粉末进行XRD测试,结果如图1(b)所示,表明产物成分为Zr0.8Ti0.2C0.95B0.05,无杂相生成。
实施例3
一种陶瓷粉体的制备,包括如下步骤:
将Zr、Ti、C、B原料粉末按Zr:Ti:C:B=0.8:0.2:0.9:0.1的比例混合均匀并压坯,得到相对密度为60%的预制块;将预制块放入石墨模具中,并将整体置于反应釜中;然后在氩气作为保护气氛,气压为1MPa的反应釜中,利用通电钨螺旋丝发热诱导预制块中各原料之间发生自蔓延燃烧反应;反应的产物冷却后经破碎研磨,得到Zr0.8Ti0.2C0.9B0.1陶瓷粉体。
对得到的粉末进行XRD测试,结果如图1(c)所示,表明产物成分为Zr0.8Ti0.2C0.9B0.1,无杂相生成。
实施例4
一种陶瓷粉体的制备,包括如下步骤:
将Zr、Ti、C、B原料粉末按Zr:Ti:C:B=0.8:0.2:0.85:0.15的比例混合均匀并压坯,得到相对密度为40%的预制块;将预制块放入石墨模具中,并将整体置于反应釜中;然后在氩气作为保护气氛,气压为10MPa的反应釜中,利用通电钨螺旋丝发热诱导预制块中各原料之间发生自蔓延燃烧反应;反应的产物冷却后经破碎研磨,得到Zr0.8Ti0.2C0.85B0.15陶瓷粉体。
对得到的粉末进行XRD测试,结果如图1(d)所示,表明产物成分为Zr0.8Ti0.2C0.85B0.15,无杂相生成。
一些实施例
为检验原料比例对陶瓷粉体化学组成的影响,即方法步骤同实施例1,仅改变原料中C和B比例,结果如下表。
表1不同原料比例的结果
实施例编号 | Zr:Ti:C:B | 陶瓷粉末组成 |
5 | 0.8:0.2:0.8:0.2 | ZrCx、TiCx、ZrB<sub>2</sub> |
6 | 0.8:0.2:0.75:0.25 | ZrCx、TiCx、ZrB<sub>2</sub> |
7 | 0.8:0.2:0.7:0.3 | ZrCx、TiCx、ZrB<sub>2</sub> |
8 | 0.8:0.2:0.65:0.35 | ZrCx、TiCx、ZrB<sub>2</sub> |
9 | 0.8:0.2:0.6:0.40 | ZrCx、TiCx、ZrB<sub>2</sub> |
10 | 0.8:0.2:0.55:0.45 | ZrCx、TiCx、ZrB<sub>2</sub> |
结果表明:当原料比例中,C<0.85且B>0.15时,合成的陶瓷粉体化学组成为ZrCx、TiCx和ZrB2,得不到单相的Zr0.8Ti0.2C1-xBx陶瓷粉体。
显然,本发明的上述实施例仅仅是为清楚地说明本发明所作的举例,而并非是对本发明的实施方式的限定,对于所属领域的普通技术人员来说,在上述说明的基础上还可以做出其它不同形式的变化或变动,这里无法对所有的实施方式予以穷举,凡是属于本发明的技术方案所引伸出的显而易见的变化或变动仍处于本发明的保护范围之列。
Claims (3)
1.一种燃烧合成制备ZrTiCB四元陶瓷粉体的方法,其特征在于,包括如下步骤:
将锆粉、钛粉、碳粉和硼粉混匀并压坯,得到相对密度为40%~60%的预制块;采用通电钨丝发热诱导预制块中各原料组分之间发生自蔓延燃烧反应;反应得到的产物冷却后研磨制得Zr0.8Ti0.2C1-xBx陶瓷粉体;其中,x取值范围为:0<x≤0.15。
2.根据权利要求1所述的方法,其特征在于,所述锆粉、钛粉、碳粉和硼粉的摩尔比为0.8:0.2:1-x:x,其中0<x≤0.15。
3.根据权利要求1所述的方法,其特征在于,所述自蔓延燃烧反应在氩气气氛且气压为0.1~10MPa条件下进行。
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