CN113651628A - 采用热压与热等静压制备硼酸铝晶须增强非金属基复合材料的方法 - Google Patents

采用热压与热等静压制备硼酸铝晶须增强非金属基复合材料的方法 Download PDF

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CN113651628A
CN113651628A CN202110701380.1A CN202110701380A CN113651628A CN 113651628 A CN113651628 A CN 113651628A CN 202110701380 A CN202110701380 A CN 202110701380A CN 113651628 A CN113651628 A CN 113651628A
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aluminum borate
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isostatic pressing
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CN113651628B (zh
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贾碧
施金良
江寒梅
王如转
万鑫
朱俊
王智远
吴慧明
吴春艳
张丹瑕
张文轩
陈星宇
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Chongqing Stiou Measurement And Control Technology Co ltd
Chongqing University of Science and Technology
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Chongqing University of Science and Technology
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Abstract

本发明公开了一种采用热压与热等静压制备硼酸铝晶须增强非金属基复合材料的方法，包括以下步骤：a.将硼酸铝晶须和非金属材料混合并球磨处理；b.将球磨后的混合料先进行真空热压烧结处理后再进行热等静压处理；经过前期的热压烧结后，复合材料已经达到了一定的相对密度，可制备出基本不含开口气孔的烧结体，再对其进行热等静压处理，主要是通过扩散蠕变机制来进一步提高相对密度，而扩散蠕变的速度与应力成正比，因此高的热等静压压力能够进一步消除体系内的气孔，愈合一些结构缺陷，从而提高材料的相对密度；而且由于热等静压是对试样施以各向同等的压力，因此烧结体的结构更加均匀。

Description

采用热压与热等静压制备硼酸铝晶须增强非金属基复合材料 的方法
技术领域
本发明涉及硼酸铝晶须增强非金属基复合材料领域，具体涉及一种采用热压与热等静压制备硼酸铝晶须增强非金属基复合材料的方法。
背景技术
硼酸铝晶须最早是由一位日本科学家研究发现的，它具有极高的杨氏模量，较大的拉伸强度和莫氏硬度。硼酸铝晶须种类繁多，其化学通式为nAl2O3·B2O3，根据烧结温度和制备方法不同，常见的有9Al2O3·2B2O3、Al2O3·B2O3、2Al2O3·B2O3这三种类型。其中9Al2O3·2B2O3的密度为2.93g cm-3，熔点1450℃左右，高硬度、高强度，不溶于酸性和碱性溶液，综合性能最佳，且价格低廉，适合大规模生产。非金属材料，如氧化铝陶瓷材料拥有高硬度、高强度、耐高温、耐磨损与耐腐蚀等优异性能，被广泛应用于结构陶瓷和耐磨元件。由于陶瓷材料固有的脆性，较差的断裂韧性限制了氧化铝陶瓷材料的工业应用。现有技术中，并没有采用硼酸铝晶须增强、增韧非金属材料(包括无机非金属材料和高分子材料)的先例。
发明内容
有鉴于此，本发明的目的在于提供一种采用热压与热等静压制备硼酸铝晶须增强非金属基复合材料的方法，使复合材料的弯曲强度、硬度及断裂韧性等性能得到提升。
本发明的采用热压与热等静压制备硼酸铝晶须增强非金属基复合材料的方法，包括以下步骤：
a.将硼酸铝晶须和非金属材料混合并球磨处理；
b.将球磨后的混合料先进行真空热压烧结处理后再进行热等静压处理；
进一步，步骤a中，所述非金属材料为包含氧化铝陶瓷在内的特种陶瓷材料；
进一步，步骤a中，所述硼酸铝晶须占复合材料的体积含量为1-50％；
进一步，步骤a中，所述硼酸铝晶须的长度为1～50μm，直径为0.05～1.0μ m；
进一步，步骤b中，热压烧结温度为1300～1650℃，烧结压力为5～60MPa；
进一步，步骤b中，热等静压的温度为1300～1500℃，压力为80～195MPa，保温时间为30～180min；
进一步，步骤a中，将硼酸铝晶须和非金属材料以及氧化锆磨球加入球磨罐中进行球磨；
进一步，步骤a中，球磨至粉体粒度小于1.0μm。
本发明的有益效果是：本发明公开的采用热压与热等静压制备硼酸铝晶须增强非金属基复合材料的方法，经过前期的热压烧结后，复合材料已经达到了一定的相对密度，可制备出基本不含开口气孔的烧结体，再对其进行热等静压处理，主要是通过扩散蠕变机制来进一步提高相对密度，而扩散蠕变的速度与应力成正比，因此高的热等静压压力能够进一步消除体系内的气孔，愈合一些结构缺陷，从而提高材料的相对密度；而且由于热等静压是对试样施以各向同等的压力，因此烧结体的结构更加均匀；再加上固溶强化作用的进一步加强，这三个方面的原因导致了复合材料弯曲强度、硬度及断裂韧性的更进一步提高。
附图说明
下面结合附图和实施例对本发明作进一步描述：
图1为试样断面的SEM图：(a)热压烧结；(b)热压烧结+热等静压烧结；
图2为（a）热压烧结(HP)和(b)热等静压烧结(HIP)下硼酸铝增强氧化铝陶瓷的EDS图；
图3为未经热等静压烧结和热等静压烧结下硼酸铝增强氧化铝陶瓷中B、O、 Al、Ti的含量表。
具体实施方式
本实施例的采用热压与热等静压制备硼酸铝晶须增强非金属基复合材料的方法，包括以下步骤：
a.将硼酸铝晶须和非金属材料混合并球磨处理；
b.将球磨后的混合料先进行真空热压烧结处理后再进行热等静压处理；经过前期的热压烧结后，复合材料已经达到了一定的相对密度，可制备出基本不含开口气孔的烧结体，再对其进行热等静压处理，主要是通过扩散蠕变机制来进一步提高相对密度，而扩散蠕变的速度与应力成正比，因此高的热等静压压力能够进一步消除体系内的气孔，愈合一些结构缺陷，从而提高材料的相对密度；而且由于热等静压是对试样施以各向同等的压力，因此烧结体的结构更加均匀；再加上固溶强化作用的进一步加强，这三个方面的原因导致了复合材料弯曲强度、硬度及断裂韧性的更进一步提高。
本实施例中，步骤a中，所述非金属材料为氧化铝陶瓷；采用硼酸铝晶须增强非金属材料；复合材料的断裂强度主要取决于材料微结构中最大的晶粒或簇的尺寸。复合材料断裂韧性的增加则主要由于晶须增韧所导致，烧结过程中液化后的硼酸铝晶须被晶粒挤出并在晶粒表面重结晶形成类似针状的晶须，同时部分晶须之间出现了桥接现象。通过由桥接晶须而导致的复合材料断裂韧性的增加。同时，由于增韧晶须而发生的裂纹偏转和桥接等也进一步提升材料断裂韧性。硼酸铝晶须种类繁多，其化学通式为nAl2O3·B2O3，根据烧结温度和制备方法不同，常见的有9Al2O3·2B2O3、Al2O3·B2O3、2Al2O3·B2O3这三种类型。其中9Al2O3·2B2O3的密度为2.93g cm-3，熔点1450℃左右，高硬度、高强度，不溶于酸性和碱性溶液，综合性能最佳，且价格低廉，适合大规模生产。陶瓷材料的磨损性能和其硬度及韧性有着密切的关系，材料的强度和韧性越大，那么材料的耐磨损性能越好。没有添加硼酸铝的氧化铝陶瓷，虽然其硬度较高，但其韧性过低，因而磨损性能较差。在氧化铝陶瓷原料体系中添加硼酸铝晶须，并在高于晶须熔点的温度上进行烧结，使其起到熔剂的作用，实现液相烧结过程。
本实施例中，步骤a中，所述硼酸铝晶须占复合材料的体积含量为1-30％；随着硼酸铝晶须体积分数的增加，氧化铝陶瓷基复合材料的弯曲强度和硬度都呈现先增加后减小的趋势，材料的断裂韧性则逐渐增加。复合材料磨损率随着硼酸铝晶须体积分数的增加呈现先降低后升高的趋势。
本实施例中，步骤a中，所述硼酸铝晶须的长度为1～50μm，直径为0.05～ 1.0μm。
本实施例中，步骤b中，热压烧结温度为1300～1650℃，烧结压力为5～ 60MPa；热等静压的温度为1380～1480℃，压力为80～195MPa，保温时间为30～180min。试样经过热等静压处理后，断面上孔隙的数量也减少了，这说明热等静压处理有助于烧结体中孔隙的排出。另外，从图中还可以看出，穿晶断裂在经过热等静压处理过后的试样中所占的比例有所增大，这说明试样晶界处的结合力进一步加强了。
本实施例中，步骤a中，将硼酸铝晶须和非金属材料以及氧化锆磨球加入球磨罐中进行球磨；
本实施例中，步骤a中，球磨至粉体粒度小于1.0μm。
实施例一
(A组)本实施例的采用热压与热等静压制备硼酸铝晶须增强非金属基复合材料的方法，包括以下步骤：
a.将硼酸铝晶须9Al2O3·2B2O3(10％体积百分比)和Al2O3(72％体积百分比)，TiB2(18％体积百分比)与氧化锆加入球磨罐中球磨至粉体粒度小于1.0μm；
b.将球磨后的混合料先进行真空热压烧结，烧结压力为36MPa，烧结温度为 1550℃得到致密体。
B组：步骤a同上；
步骤b：将球磨后的混合料先进行真空热压烧结，烧结压力为36MPa，烧结温度为1550℃得到致密体，再将致密体在压力为150MPa，温度为1430℃的环境下热等静压处理60分钟。
将实施例一获得的试样和对比例的试样进行测试：A组：平均晶粒尺寸1.2 μm，断面孔隙较多；B组：平均晶粒尺寸2.3μm，断面孔隙较少。如图1所示，试样经过150MPa的热等静压处理后，平均晶粒尺寸从1.2μm长大至2.3μm。进行热等静压处理，相当于延长了烧结时间，尽管温度较低只有1430℃，但140 MPa的烧结压力提高了材料体系内各物质迁扩散速率和晶界移动速率，从而导致了晶粒的长大。从图中还可以看出，试样经过热等静压处理后，断面上孔隙的数量也减少了，这说明热等静压处理有助于烧结体中孔隙的排出。另外，从图中还可以看出，穿晶断裂在经过热等静压处理过后的试样中所占的比例有所增大，这说明试样晶界处的结合力进一步加强了。
图2为热压烧结(HP)和(b)热等静压烧结(HIP)下硼酸铝增强氧化铝陶瓷的EDS图；图3为未经热等静压烧结和热等静压烧结下硼酸铝增强氧化铝陶瓷中B、O、Al、Ti的含量表；从图2和图3可以看出，经过热等静压处理后，粘结相硼酸铝中固溶的钛元素增多了。这说明热等静压处理增强了硼酸铝相的固溶强化作用。
热压和热等静压烧结处理试样的性能：
Figure RE-GDA0003311041430000051
从上表可以看出，经过热等静压处理后，陶瓷的相对密度从98.76％上升到99.81％。经过前期的热压烧结后，材料已经达到了一定的相对密度，再对其进行热等静压处理，主要是通过扩散蠕变机制来进一步提高相对密度，而扩散蠕变的速度与应力成正比，因此高的热等静压压力能够进一步消除体系内的气孔，愈合一些结构缺陷，从而提高材料的相对密度；而且由于热等静压是对试样施以各向同等的压力，因此烧结体的结构更加均匀；再加上固溶强化作用的进一步加强，这三个方面的原因导致了材料弯曲强度、硬度及断裂韧性的提高。
实施例二
本实施例的采用热压与热等静压制备硼酸铝晶须增强非金属基复合材料的方法，包括以下步骤：
a.将硼酸铝晶须9Al2O3·2B2O3(20％体积百分比)和Al2O3(67％体积比)，TiB2(13％体积比)与氧化锆加入球磨罐中球磨至粉体粒度小于1.0μm；所述硼酸铝晶须的长度为5μm，直径为0.4μm；
b.将球磨后的混合料先进行真空热压烧结，烧结压力为5MPa，烧结温度为 1300℃得到致密体，再将致密体在压力为80MPa，温度为1380℃的环境下热等静压处理60分钟。
实施例三
本实施例的采用热压与热等静压制备硼酸铝晶须增强非金属基复合材料的方法，包括以下步骤：
a.将硼酸铝晶须9Al2O3·2B2O3(10％体积百分比)和Al2O3(80％体积比)，TiB2(10％体积比)与氧化锆加入球磨罐中球磨至粉体粒度小于1.0μm；所述硼酸铝晶须的长度为10μm，直径为0.8μm；
b.将球磨后的混合料先进行真空热压烧结，烧结压力为60MPa，烧结温度为1650℃得到致密体，再将致密体在压力为195MPa，温度为1480℃的环境下热等静压处理30分钟。
实施例四
本实施例的采用热压与热等静压制备硼酸铝晶须增强非金属基复合材料的方法，包括以下步骤：
a.将硼酸铝晶须9Al2O3·2B2O3(30％体积百分比)和Al2O3(50％体积比)，TiB2(20％体积比)与氧化锆加入球磨罐中球磨至粉体粒度小于1.0μm；所述硼酸铝晶须的长度为50μm，直径为1.0μm；
b.将球磨后的混合料先进行真空热压烧结，烧结压力为36MPa，烧结温度为 1550℃得到致密体，再将致密体在压力为170MPa，温度为1450℃的环境下热等静压处理180分钟。
最后说明的是，以上实施例仅用以说明本发明的技术方案而非限制，尽管参照较佳实施例对本发明进行了详细说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的宗旨和范围，其均应涵盖在本发明的权利要求范围当中。

Claims (8)

1.一种采用热压与热等静压制备硼酸铝晶须增强非金属基复合材料的方法，其特征在于：包括以下步骤：
a.将硼酸铝晶须和非金属材料混合并球磨处理；
b.将球磨后的混合料先进行真空热压烧结处理后再进行热等静压处理。
2.根据权利要求1所述的采用热压与热等静压制备硼酸铝晶须增强非金属基复合材料的方法，其特征在于：步骤a中，所述非金属材料为氧化铝陶瓷。
3.根据权利要求2所述的采用热压与热等静压制备硼酸铝晶须增强非金属基复合材料的方法，其特征在于：步骤a中，所述硼酸铝晶须占复合材料的体积含量为1-50％。
4.根据权利要求3所述的采用热压与热等静压制备硼酸铝晶须增强非金属基复合材料的方法，其特征在于：步骤a中，所述硼酸铝晶须的的长度为1～50μm，直径为0.05～1.0μm。
5.根据权利要求1所述的采用热压与热等静压制备硼酸铝晶须增强非金属基复合材料的方法，其特征在于：步骤b中，热压烧结温度为1300～1650℃，烧结压力为5～60MPa。
6.根据权利要求5所述的采用热压与热等静压制备硼酸铝晶须增强非金属基复合材料的方法，其特征在于：步骤b中，热等静压的温度为1300～1500℃，压力为80～195MPa，保温时间为30～180min。
7.根据权利要求1所述的采用热压与热等静压制备硼酸铝晶须增强非金属基复合材料的方法，其特征在于：步骤a中，将硼酸铝晶须和非金属材料以及氧化锆磨球加入球磨罐中进行球磨。
8.根据权利要求7所述的硼酸铝晶须增强非金属基复合材料的制备方法，其特征在于：步骤a中，球磨至粉体粒度小于1.0μm。
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