CN105924177A - 一种碳化硼基复相陶瓷的热压-反应烧结制备方法 - Google Patents
一种碳化硼基复相陶瓷的热压-反应烧结制备方法 Download PDFInfo
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Abstract
本发明涉及一种碳化硼基复相陶瓷的热压‑反应烧结制备方法,属于复相陶瓷材料制备领域。原料中各成分比例如下:铝15~25%,氧化硼20~35%,石墨1.2~3%,碳化硼40~62%;所述方法为:将原料依次加入,然后进行球磨混合、干燥和过筛,制成混合粉体;将混合粉放入石墨模具进行热压‑反应烧结,通氩气或氮气,≤1000℃升温速率为18~22℃/min;>1000℃升温速率为13~18℃/min;升至1300~1400℃施加压力至35~40MPa,保持压力至烧结结束;升温至1600~1800℃保温20~40min,烧结结束脱模得到所述复相陶瓷。所述方法烧结效率高,烧结温度低;制得的复相陶瓷致密度高,力学性能好。
Description
技术领域
本发明涉及一种碳化硼基复相陶瓷的热压-反应烧结制备方法,属于复相陶瓷材料制备领域。
背景技术
碳化硼(B4C)陶瓷具有密度低、熔点高、化学稳定性强以及耐磨性好等优良性能,尤其是其高硬度、低密度使其在许多领域的应用尤为突出,比如可用于装甲车的披挂装甲和航空器的防护面板等。但是纯碳化硼过高的烧结成本和材料本身较大的脆性限制了它的广泛应用,因此对碳化硼这两个方面的改进迫在眉睫。
在研制碳化硼基复相陶瓷材料的过程中,碳化硼-氧化铝(B4C-Al2O3)复相陶瓷材料是众多从事B4C材料科研工作者们的研究重点。但纵观国内外文献,在制备B4C-Al2O3复相陶瓷材料的过程中,多数方法是将Al2O3作为单一相直接引入到原料中,制备成混合粉体后再进行烧结,并且烧结工艺也主要集中在单纯的无压烧结、热压烧结等传统的烧结方式。将高温还原合成法引入到B4C基复相陶瓷材料的制备,还未见应用。
发明内容
针对现有技术存在的缺陷,本发明目的在于提供一种碳化硼基复相陶瓷的热压-反应烧结制备方法,所述制备方法采用热压-反应烧结,同时添加铝(A1)、氧化硼(B2O3)、石墨(C)来对碳化硼(B4C)的热压烧结行为进行改善。
为实现本发明的目的,提供以下技术方案。
一种碳化硼基复相陶瓷的热压-反应烧结制备方法,步骤如下:
(1)成分配比:称量原料后,依次进行球磨混合、干燥和过筛,制成混合粉体;以所述原料的总体质量为100%计,其中,各组成成分及其质量百分数如下:
所述原料为:粒度为2~5μm的铝粉,粒度为1~150μm的氧化硼粉,粒度为0.2~0.3μm的石墨粉,粒度为1~5μm的碳化硼粉;铝粉的纯度为99.99%,氧化硼粉的纯度为99.5%,石墨粉的纯度为99.9%,碳化硼粉的纯度为99%;
球磨的球料比为5﹕1,球磨机转速为300r/min,球磨时间为2.5h;介质为无水乙醇,液料体积百分比为3﹕1,球磨混合后,采用旋转蒸发仪将其中的无水乙醇与固体原料分离;
将原料置于恒温鼓风干燥箱中于70℃静置48h进行干燥;
干燥后的原料用300目的标准试验筛筛分。
(2)将混合粉体放入石墨模具进行热压-反应烧结,热压-反应烧结全程通入氩气或氮气,其他反应条件为:在≤1000℃时,升温速率为18℃/min~22℃/min;在>1000℃时,升温速率为13℃/min~18℃/min;在温度升至1300℃~1400℃时开始施加压力,直至达到35MPa~40MPa,并保持所述压力至烧结结束,升温至1600℃~1800℃保温20min~40min热压-反应烧结结束,脱模,得到本发明所述的一种碳化硼基复相陶瓷。
有益效果
1.本发明提供了一种碳化硼基复相陶瓷的热压-反应烧结制备方法,所述制备方法选用易于得到且价格低廉的原材料,制备成本低;
2.本发明提供了一种碳化硼基复相陶瓷的热压-反应烧结制备方法,所述制备方法将能够引发高温还原反应的原料加入到纯B4C中,再进行烧结;所述高温还原反应必须符合以下几点要求:
(1)达到烧结温度前的温度条件足以使反应发生;
(2)反应过程中放出大量的热;
(3)反应的主产物为碳化硼和氧化铝。
综上所述,本发明以B2O3、Al和C为添加剂,按反应方程式的配比制成复合添加剂,与纯B4C粉体以不同的比例混合;烧结过程中产生高放热反应,使混合粉体颗粒产生活化,降低烧结温度;
3.本发明提供了一种碳化硼基复相陶瓷的热压-反应烧结制备方法,所述制备方法在1300℃~1400℃时开始加压,这是因为1300℃~1400℃是反应终产物始于生成的温度,发生剧烈放热反应:2B2O3+C+Al→B4C+Al2O3,如若过早加压,会将正处于液体状态的反应物Al、B2O3从模具中挤出;上述加压方式制备碳化硼基复相陶瓷时,机械压力越大,越有利于降低所述复相陶瓷的气孔率,从而获得高致密度的产品,但是限于石墨模具的承压极限一般为45MPa,为了保证模具的使用寿命和烧结时的安全,因此将压力限定为35MPa~40MPa;
4.本发明提供了一种碳化硼基复相陶瓷的热压-反应烧结制备方法,所述制备方法制备出的碳化硼基复相陶瓷致密度高,性能好:硬度高,可达92HRA~95HRA;抗弯强度大,可达400MPa以上;断裂韧性高,可达3.5MPa·m1/2~5.2MPa·m1/2;相对密度大,可达98%T.D.左右;
具体实施方式
下面对本发明的优选实施方式做出详细说明。
以下实施例中:
原料:铝粉的粒度为2~5μm,纯度为99.99%;氧化硼粉的粒度为1~150μm,纯度为99.5%;石墨粉的粒度为0.2~0.3μm,纯度为99.9%;碳化硼粉的粒度为1~5μm,纯度为99%;
R-C-ZKQY-07型热压烧结炉购自上海辰荣电炉有限公司;
石墨模具采用北京三业碳素有限公司加工的石墨模具,承压极限为45MPa;
所述无水乙醇为分析纯产品。
实施例1
一种碳化硼基复相陶瓷的热压-反应烧结制备方法,所述方法步骤如下:
(1)称取原料如下:以原料的总体质量为100%计,其中,各组成成分及其质量百分数如下:铝18.53%,氧化硼23.89%,石墨2.06%,碳化硼55.52%;
称量原料后,将原料在球磨机中进行球磨混合,球磨的球料比为5﹕1,球磨机转速为300r/min,球磨时间为2.5h;介质选用无水乙醇,液料体积百分比为3﹕1,球磨混合后,采用旋转蒸发仪将其中的无水乙醇与固体原料分离;将固体原料置于恒温鼓风干燥箱中于70℃静置48h进行干燥;将干燥后的原料用300目的标准试验筛筛分,制成混合粉体;
(2)将混合粉体放入R-C-ZKQY-07型热压烧结炉的石墨模具中进行热压-反应烧结,当真空计显示0.1Pa以下时,开始通入氩(Ar)气作为保护性气体,至炉内达到规定气压5MPa时关闭气阀,同时打开加热电源,进行加热,当温度达到1000℃,升温速率为15℃/min;1050℃以上时,升温速率为10℃/min;当温度达到1300℃时,开始缓慢加压,约10min后达到预设压力35MPa,保压至热压-反应烧结过程结束;石墨模具中的反应物温度达到1750℃时保温30min,然后,关闭加热开关,石墨模具中的反应物随炉冷却,冷却至300℃时,卸压,待炉内温度冷却至室温时,取出石墨模具,将产物脱模,用300#砂纸磨掉产物表面碳纸,即得最终产物。
将最终产品进行如下检测:
(1)物相组成检测:用X射线衍射仪(X'Pert PRO MPD,荷兰PANalytical公司)分析最终产品的物相组成,采用CuKa辐射。经检测可知,最终产品的相组成如下:主相为B4C,第二相为Al2O3,AlB12C2、Al18B4O33、Al4C3、AlB2和AlB12,为本发明所述的一种碳化硼基复相陶瓷;
(2)性能检测:最终产品的体积密度利用Archimedes法进行测试,并根据最终产品相应的理论密度计算样品的相对密度(谢志鹏.结构陶瓷[M].北京:清华大学出版社,2011),采用洛氏硬度测试表征最终产品硬度,最终产品的抗弯强度采用三点弯曲法测试,在电子万能试验机(WDW-E100D,济南试验机厂)上进行测量。采用SENB法在万能试验机上(WDW-E100D,济南试验机厂)测量最终产品的断裂韧性。经检测可知,最终产品性能如下:体积密度为2.83g/cm3,相对密度为98.3%,洛式硬度为94HRA,抗弯强度为440MPa,断裂韧性为4.4MPa·m1/2。
实施例2
一种碳化硼基复相陶瓷的热压-反应烧结制备方法,所述方法步骤如下:
(1)称取原料如下:以原料的总体质量为100%计,其中,各组成成分及其质量百分数如下:铝15.89%,氧化硼20.47%,石墨1.76%,碳化硼61.88%;其余同实施例1步骤(1);
(2)通入氮气作为保护性气体,石墨模具中的反应物温度达到1650℃时保温40min,自然冷却;其余同实施例1步骤(2)。
将最终产品进行如下检测:
(1)物相组成检测:用X射线衍射仪(X'Pert PRO MPD,荷兰PANalytical公司)分析最终产品的物相组成,采用CuKa辐射。经检测可知,最终产品的相组成如下:主相为B4C,第二相为Al2O3,AlB12C2、Al18B4O33、Al4C3、AlB2和AlB12,为本发明所述的一种碳化硼基复相陶瓷;
(2)性能检测:最终产品的体积密度利用Archimedes法进行测试,并根据最终产品相应的理论密度计算样品的相对密度(谢志鹏.结构陶瓷[M].北京:清华大学出版社,2011),采用洛氏硬度测试表征最终产品硬度,最终产品的抗弯强度采用三点弯曲法测试,在电子万能试验机(WDW-E100D,济南试验机厂)上进行测量。采用SENB法在万能试验机上(WDW-E100D,济南试验机厂)测量最终产品的断裂韧性。经检测可知,最终产品性能如下:体积密度为2.78g/cm3,相对密度为98%,洛式硬度为95HRA,抗弯强度为420MPa,断裂韧性为4.2MPa·m1/2。
Claims (1)
1.一种碳化硼基复相陶瓷的热压-反应烧结制备方法,其特征在于:所述方法步骤如下:
(1)称量原料后,依次进行球磨混合、干燥和过筛,制成混合粉体;
以原料总体质量为100%计,各组成成分及其质量百分数如下:
(2)将混合粉体放入石墨模具进行热压-反应烧结,热压-反应烧结全程通入氩气或氮气,其他反应条件为:在≤1000℃时,升温速率为18℃/min~22℃/min;在>1000℃时,升温速率为13℃/min~18℃/min;在温度升至1300℃~1400℃时开始施加压力,直至达到35MPa~40MPa,并保持所述压力至烧结结束,升温至1600℃~1800℃保温20min~40min,热压-反应烧结结束,脱模,得到所述的一种碳化硼基复相陶瓷。
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