CN108409333B - 一种AlMgB14-TiB2/Ti梯度功能复合材料及其制备方法 - Google Patents

一种AlMgB14-TiB2/Ti梯度功能复合材料及其制备方法 Download PDF

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CN108409333B
CN108409333B CN201810247975.2A CN201810247975A CN108409333B CN 108409333 B CN108409333 B CN 108409333B CN 201810247975 A CN201810247975 A CN 201810247975A CN 108409333 B CN108409333 B CN 108409333B
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庄蕾
徐春林
潘毅
柳青松
王家珂
孙运腾
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Yangzhou Polytechnic Institute
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Abstract

一种AlMgB14‑TiB2/Ti梯度功能复合材料及其制备方法，属于复合材料制备的技术领域。该梯度材料一侧为Ti金属材料，另一侧为AlMgB14陶瓷材料，在AlMgB14陶瓷粉末中加入TiB2粉末作为中间层，中间层数为3层，沿富Ti方向到富AlMgB14方向，材料硬度、强度显著提高，抗氧化以及抗高温性能提高，耐磨损性能以及弹性模量都逐渐提高；沿富AlMgB14方向到富Ti方向，韧性、导电率、导热率都得到显著提高。通过TiB2材料的过渡，增强了AlMgB14和Ti之间的结合作用，提高了材料的韧性、抗剪切强度和压溃强度。制备方法采用的碳化硅陶瓷模具使试样坯料产生均匀和集中的电流分布，保证了粉体间界面的反应强度,促进了扩散烧结过程，缩短了试样的制备时间。

Description

一种AlMgB14-TiB2/Ti梯度功能复合材料及其制备方法
技术领域
本发明属于复合材料制备的技术领域，涉及一种AlMgB14-TiB2/Ti梯度功能复合材料及其制备方法，具体的说是涉及一种通过脉冲电场作用下进行反应扩散烧结方法制备的AlMgB14-TiB2/Ti梯度功能复合材料。
背景技术
金属Ti具有高比强度、高韧性和减摩性等优点，由于其与硼化物具有良好的亲和性而成为理想的高级韧性增强材料，AlMgB14材料具有超高硬度、高耐磨性能及良好的化学稳定性，适用于制造军事装备和极端力学条件下的机械装备，但由于AlMgB14材料韧性较低，限制了其应用范围。
发明内容
本发明的目的是针对上述现有技术中存在的不足，提出一种AlMgB14-TiB2/Ti梯度功能复合材料及其制备方法，以AlMgB14和Ti为基础材料，以TiB2为过渡材料，通过脉冲电场作用进行反应扩散烧结制备成梯度功能材料，该材料可有效解决上述技术中的缺陷，材料的表面硬度、抗断裂韧性和抗弯强度可得到大幅度提高，可进一步提升材料的耐热性、隔热性和高温抗氧化性能。
本发明的技术方案是：一种AlMgB14-TiB2/Ti梯度功能复合材料，包括Ti金属粉末和AlMgB14陶瓷粉末；其特征在于：在所述AlMgB14陶瓷粉末中加入TiB2粉末混合形成中间层，所述Ti金属粉末和AlMgB14陶瓷粉末作为外层分别设置在中间层的两侧，在脉冲电场作用下压制烧结成型。
所述Ti金属粉末和AlMgB14陶瓷粉末的粒径为30～50μm。
所述TiB2粉末的粒径不大于200nm。
所述中间层的层数不少于3层。
一种AlMgB14-TiB2/Ti梯度功能复合材料的制备方法，包括如下制备步骤：
(1)将AlMgB14陶瓷粉末、Ti金属粉末、TiB2粉末在乙醇中进行超声波分散处理1h；
(2)将超声波分散后的上述各粉末置于干燥箱中干燥2h；
(3)取干燥后的TiB2粉末加入至AlMgB14陶瓷粉末中均匀混合，并将其置于刚玉球磨罐中球磨10h形成AlMgB14-TiB2混合粉末；
(4)依次将Ti金属粉末、AlMgB14-TiB2混合粉末、AlMgB14陶瓷粉末堆叠于碳化硅模具管中；
(5)将碳化硅模具管置于反应炉中的上石墨压头和下石墨压头之间并施加压力，压制成柱状坯料；
(6)将反应炉内抽真空至10-3～10-4Pa，接通电源调节脉冲电流频率至40～50Hz，将电流调节至1000～1600A，保持10～15min，烧结完成后将电流缓慢调节至零；
(7)将柱状坯料随炉冷却至室温即成AlMgB14-TiB2/Ti梯度功能复合材料。
步骤(3)中所述AlMgB14-TiB2混合粉末分为三层，从下往上每层中的TiB2质量分数分别为20～30%、40～50%和60～70%(修改)。
所述碳化硅模具管的内径为20mm，壁厚为1mm。
本发明的有益效果为：本发明提供的一种AlMgB14-TiB2/Ti梯度功能复合材料及其制备方法，本发明制备方法采用的碳化硅陶瓷模具使试样坯料产生均匀和集中的电流分布，保证了粉体间界面的反应强度，促进了扩散烧结过程，缩短了试样的制备时间。界面粉体在瞬间强脉冲电场的作用下快速产生的反应热使结合界面区加热和局部熔化，形成元素互扩散和化合，在压力的辅助作用下快速形成固相烧结，AlMgB14陶瓷到Ti金属的连续过渡，使材料既具有良好的韧性、抗剪切强度和压溃强度，又具有良好的耐热、隔热、高强及高温抗氧化性，同时由于中间成分的连续变化，消除了材料中的宏观界面，整体材料表现出良好的热应力缓和特性，使之能在超高温、大温差、高速热流冲击等苛刻环境条件下使用。特别适用于航天飞机的机身、燃烧室内壁等以及涡轮发动机、高效燃气轮机等特殊场合。
附图说明
图1 为本发明制备装置示意图。
图2 为本发明梯度结构示意图。
图中：上铜电极1、下铜电极2、上石墨压头3、下石墨压头4、碳化硅模具管5、直流脉冲电源6、梯度复合材料7、轴向压力8、石墨模具9。
具体实施方式
下面结合附图对本发明作进一步说明：
一种AlMgB14-TiB2/Ti梯度功能复合材料，包括Ti金属粉末和AlMgB14陶瓷粉末；其特征在于：在所述AlMgB14陶瓷粉末中加入TiB2粉末混合形成中间层，所述Ti金属粉末和AlMgB14陶瓷粉末作为外层分别设置在中间层的两侧，在脉冲电场作用下压制烧结成型。Ti金属粉末和AlMgB14陶瓷粉末的粒径为30～50μm；TiB2粉末的粒径不大于200nm；中间层的层数不少于3层。
如图1-2所示，一种AlMgB14-TiB2/Ti梯度功能复合材料的制备方法，包括如下制备步骤：
(1)将AlMgB14陶瓷粉末、Ti金属粉末、TiB2粉末在乙醇中进行超声波分散处理1h；
(2)将超声波分散后的上述各粉末置于干燥箱中干燥2h；
(3)取干燥后的TiB2粉末加入至AlMgB14陶瓷粉末中均匀混合，并将其置于刚玉球磨罐中球磨10h形成AlMgB14-TiB2混合粉末；
(4)依次将Ti金属粉末、AlMgB14-TiB2混合粉末、AlMgB14陶瓷粉末堆叠于碳化硅模具管5中；
(5)将碳化硅模具管5置于反应炉中的上石墨压头3和下石墨压头4之间并施加压力，压制成柱状坯料；
(6)将反应炉内抽真空至10-3～10-4Pa，接通电源调节脉冲电流频率至40～50Hz，将电流调节至1000～1600A，保持10～15min，烧结完成后将电流缓慢调节至零；
(7)将柱状坯料随炉冷却至室温即成AlMgB14-TiB2/Ti梯度功能复合材料。
步骤(3)中AlMgB14-TiB2混合粉末分为三层，从下往上每层中的TiB2质量分数分别为20～30%、40～50%和60～70%；碳化硅模具管5的内径为20mm，壁厚为1mm。
实施例1
分别将质量分数为20%、40%和60%的TiB2加入AlMgB14中混合均匀，在刚玉球磨罐中球磨10h备用。在模具中，由下至上依次放置Ti金属粉末、AlMgB14与TiB2的混合粉、AlMgB14陶瓷粉末，中间层为3层。将模具放置压力机中，采用15MPa压力压制成柱状坯料。AlMgB14陶瓷粉末和Ti金属粉末的粒径尺寸为30～50μm，TiB2粉末的粒径尺寸为200nm，粉体在混合之前，在乙醇中进行超声波分散处理1小时，在干燥箱中干燥2小时。
如图1所示，将坯料置于电极之间的碳化硅模具管内，将脉冲频率40Hz的电流升至1500A，保持10min后降至1200A，保持15min，最后关闭电源，试样随炉冷却至室温。整个过程炉内真空度为2×10-4Pa，施加双向压力40MPa，试样自然冷却后从模具中取出。梯度功能复合材料的平均表面硬度达到35.8GPa，断裂韧性为23.15MPa.m0.5，抗弯强度1912MPa，表面摩擦系数为0.12。
实施例2
分别将质量分数为30%、50%和70%的TiB2加入AlMgB14中混合均匀，在刚玉球磨罐中球磨10h备用。在模具中，由下至上依次放置Ti金属粉末、AlMgB14与TiB2的混合粉、AlMgB14陶瓷粉末，中间层为3层。将模具放置压力机中，采用15MPa压力压制成柱状坯料。AlMgB14陶瓷粉末和Ti金属粉末的粒径尺寸为30～50μm，TiB2粉末的粒径尺寸为200nm，粉体在混合之前，在乙醇中进行超声波分散处理1小时，在干燥箱中干燥2小时。
如图1所示，将坯料置于电极之间的碳化硅模具管内，将脉冲频率50Hz的电流升至1500A，保持10min后降至1300A，保持15min，最后关闭电源，试样随炉冷却至室温。整个过程炉内真空度为2×10-4Pa，施加双向压力50MPa，试样自然冷却后从模具中取出。梯度功能复合材料的平均表面硬度达到38.5GPa，断裂韧性为29.76MPa.m0.5，抗弯强度1970MPa，表面摩擦系数为0.1。

Claims (2)

1.一种AlMgB14-TiB2/Ti梯度功能复合材料的制备方法，原料包括Ti金属粉末、AlMgB14陶瓷粉末和TiB2粉末，其特征在于：所述Ti金属粉末和AlMgB14陶瓷粉末的粒径为30～50μm，在所述AlMgB14陶瓷粉末中加入TiB2粉末混合形成中间层，所述TiB2粉末的粒径不大于200nm；具体制备步骤如下：
(1)将AlMgB14陶瓷粉末、Ti金属粉末、TiB2粉末在乙醇中进行超声波分散处理1h；
(2)将超声波分散后的上述各粉末置于干燥箱中干燥2h；
(3)取干燥后的TiB2粉末加入至AlMgB14陶瓷粉末中均匀混合，并将其置于刚玉球磨罐中球磨10h形成AlMgB14-TiB2混合粉末；
(4)由下至上依次将Ti金属粉末、AlMgB14-TiB2的混合粉末、AlMgB14陶瓷粉末堆叠于碳化硅模具管(5)中，其中，AlMgB14-TiB2混合粉末分为三层，由下至上每层中的TiB2质量分数分别为60～70%、40～50%和20～30%；
(5)将碳化硅模具管(5)置于反应炉中的上石墨压头(3)和下石墨压头(4)之间并施加压力，压制成柱状坯料；
(6)将反应炉内抽真空至10-3～10-4Pa，接通电源调节脉冲电流频率至40～50Hz，将电流调节至1000～1600A，保持10～15min，烧结完成后将电流缓慢调节至零；
(7)随炉冷却至室温即成AlMgB14-TiB2/Ti梯度功能复合材料。
2.根据权利要求1所述的一种AlMgB14-TiB2/Ti梯度功能复合材料的制备方法，其特征在于：所述碳化硅模具管(5)的内径为20mm，壁厚为1mm。
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