CN116217240B - 一种织构化的梯度陶瓷复合材料及其制备方法和应用 - Google Patents

一种织构化的梯度陶瓷复合材料及其制备方法和应用 Download PDF

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CN116217240B
CN116217240B CN202211557114.7A CN202211557114A CN116217240B CN 116217240 B CN116217240 B CN 116217240B CN 202211557114 A CN202211557114 A CN 202211557114A CN 116217240 B CN116217240 B CN 116217240B
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郭伟明
顾乾坤
周义
林华泰
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Guangdong University of Technology
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Abstract

本发明属于无机材料制备技术领域，公开了一种织构化的梯度陶瓷复合材料及其制备方法和应用。所述织构化的梯度陶瓷复合材料由***为环状、向心织构的SiAlON陶瓷和内部为柱状、随机织构的Si3N4陶瓷组成，是将柱状的Si3N4陶瓷预烧结体置于环状的SiAlON陶瓷预烧结体中，在1750～1800℃，同时加压30～40MPa，通过放电等离子烧结制得。该方法制备的织构化的梯度陶瓷复合材料可以实现不同陶瓷材料之间的结合，同时织构过后的陶瓷材料的性能出现显著的各向异性，在垂直棒状晶粒的方向具有更高的硬度、抗弯强度、断裂韧性、断裂能和耐磨性；在平行棒状晶粒方向具有更高的弹性模量、蠕变阻力和热导率。

Description

一种织构化的梯度陶瓷复合材料及其制备方法和应用
技术领域
本发明属于无机材料技术领域，更具体地，涉及一种织构化的梯度陶瓷复合材料及其制备方法和应用。
背景技术
织构化陶瓷材料是通过使陶瓷内部的棒状晶粒重新定向排列，使陶瓷材料的性能出现显著的各向异性，在垂直棒状晶粒的方向具有最高的硬度、抗弯强度、断裂韧性、断裂能和耐磨性；在平行棒状晶粒方向具有最高的弹性模量、蠕变阻力和热导率；梯度陶瓷材料是指成分与性能沿某一方向呈梯度变化的陶瓷材料。不同界面上的陶瓷材料，呈现出不同的性能，可以使一侧陶瓷具有更高的硬度、耐磨性和耐高温性能，另一侧的陶瓷具有更高的断裂韧性。梯度陶瓷可通过粉末冶金、焊接等方法制备。用这两种方法制备的梯度陶瓷，不同成分区域之间的界面附近常会有应力集中或者气孔、裂纹等缺陷，严重损害材料的力学性能。
发明内容
为了解决现有技术中存在的缺点和不足之处，本发明首要目的在于提供一种织构化的梯度陶瓷复合材料。
本发明的另一目的在于提供上述织构化的梯度陶瓷复合材料的制备方法。
本发明的再一目的在于提供上述织构化的梯度陶瓷复合材料的应用。
本发明的目的通过下述技术方案来实现：
一种织构化的梯度陶瓷复合材料，所述织构化的梯度陶瓷复合材料是由***为环状、向心织构的SiAlON陶瓷和内部为柱状、随机织构的Si3N4陶瓷组成，是将柱状的Si3N4陶瓷预烧结体置于环状的SiAlON陶瓷预烧结体中，在1750～1800℃，同时加压30～40MPa，通过放电等离子烧结制得。
优选地，所述织构化的梯度陶瓷复合材料的相对密度大于98％，***环状、向心织构的SiAlON陶瓷的硬度为18～22GPa，断裂韧性为4～7MPa·m1/2，抗弯强度为10～14MPa；内部柱状、随机织构的Si3N4陶瓷的硬度为15～18GPa，断裂韧性为6～8MPa·m1/2，抗弯强度为12～16MPa。
优选地，所述环状的SiAlON预烧结体是将α-Si3N4、Y2O3、Al2O3和AlN粉体混合干燥后，混合粉体在1450～1650℃，压力为25～35MPa，保护气氛为N2，通过热压烧结或放电等离子烧结制得。
优选地，按照α-Si3N4粉体的总质量为100％计算，Al2O3的质量百分比为2～5％，AlN的质量百分比为5～8％，Y2O3的质量百分比为3～5％。
优选地，所述柱状的Si3N4预烧结体是将α-Si3N4、Y2O3和Al2O3粉体混合干燥后，混合粉体在1450～1650℃，压力为25～35MPa，保护气氛为N2，通过热压烧结或放电等离子烧结制得。
优选地，按照α-Si3N4粉体的总质量为100％计算，Al2O3的质量百分比为5～10％，Y2O3的质量百分比为5～10％。
所述的织构化的梯度陶瓷复合材料的制备方法，包括以下步骤：
S1.将α-Si3N4、Y2O3、Al2O3和AlN粉体混合干燥后，置于石墨模具中，通过热压烧结或放电等离子烧结，升温至1450～1650℃，烧结压力为25～35MPa，保护气氛为N2，冷却后取出脱模，制得环状的SiAlON陶瓷预烧结体；
S2.将α-Si3N4、Y2O3、Al2O3粉体混合干燥后，置于石墨模具中，通过热压烧结或放电等离子烧结，升温至1450～1650℃，烧结压力为25～35MPa，保护气氛为N2，冷却后取出脱模，制得柱状的Si3N4陶瓷预烧结体；
S3.将环状的SiAlON陶瓷预烧结体和柱状的Si3N4陶瓷预烧结体置于同一柱状模具中，柱状的Si3N4陶瓷预烧结体置于环状的SiAlON陶瓷预烧结体内，二者中间留有空位，通过放电等离子烧结，先在3～5MPa压力下以130～150℃/min的速率升温，升至1000～1200℃开始充氮气并且逐渐增加压力，以同样的升温速率升温到1750～1800℃，同时加压达到30～40MPa，并保压保温8～10min，随后以130～150℃/min的降温速率降温，冷却后取出，制得织构化的梯度陶瓷复合材料。
优选地，步骤S1和S2中所述热压烧结的程序为：以10～14℃/min的速率升温至800～1000℃开始充氮气并且开始加压，继续以6～8℃/min的速率升温至1450～1650℃，同时压力升至25～35MPa；升温程序执行完毕后保温保压3～7min；再以10～12℃/min的速率降温至1000～1200℃泄压完毕，降温至750～850℃随炉降温；所述放电等离子烧结的程序为：以130～150℃/min的速率升温至1000～1200℃开始充氮气并且开始加压，继续将温度升至1450～1650℃，同时压力升至25～35MPa；升温程序执行完毕后保温保压3～7min；然后以80～100℃/min的速率降温至1000～1200℃泄压完毕，降温至750～850℃随炉降温。
优选地，步骤S1和S2中所述α-Si3N4的纯度均为95～100％，粒径为<0.2μm；所述Al2O3的纯度为99.9～100％，粒径为<0.2μm；所述AlN的纯度为99.9～100％，粒径为3～5μm；所述Y2O3的纯度为99.9～100％，粒径为3～6μm。
所述的织构化的梯度陶瓷复合材料在切削难加工材料、航空航天耐磨零部件或轴承制备领域中的应用。
本发明的织构化的梯度陶瓷复合材料的制备过程中在模具内Si3N4陶瓷柱状预烧结体置于SiAlON陶瓷环状预烧结体内，二者中间留有空位，烧结过程中陶瓷预烧结体受到机械压力分别向外向内流动，填充中间的空位，直至二者完全烧结到一起。本发明的织构化陶瓷复合材料是将环状预烧结体与柱状预烧结体同心置于模具中，在烧结过程中加热加压，使得陶瓷复合材料发生高温塑性变形，诱导晶粒旋转，***的环状生坯在晶粒旋转后发生向心织构，内部的柱状生坯发生随机织构，环状预烧结体与柱状预烧结体在烧结过程中分别向内向外流动，直至结合到一起，获得织构化的梯度陶瓷复合材料。
与现有技术相比，本发明具有以下有益效果：
1.本发明的织构化的梯度陶瓷复合材料中通过使材料内部的Si3N4和SiAlON棒状晶粒重新定向排列，使复合陶瓷材料的性能出现显著的各向异性，在垂直Si3N4和SiAlON棒状晶粒的方向均具有更高的硬度、抗弯强度、断裂韧性、断裂能和耐磨性；在平行Si3N4和SiAlON棒状晶粒方向均具有更高的弹性模量、蠕变阻力和热导率。
2.本发明的织构化的梯度陶瓷复合材料是将SiAlON陶瓷预烧体与Si3N4陶瓷预烧体通过放电等离子烧结复合，使得织构化的梯度复合陶瓷材料兼具SiAlON陶瓷材料的耐磨性和耐高温性能以及Si3N4陶瓷材料的断裂韧性。
说明附图
图1是本发明的陶瓷预烧结体在模具内的位置及陶瓷复合材料的织构方式示意图。
具体实施方式
下面结合具体实施例进一步说明本发明的内容，但不应理解为对本发明的限制。若未特别指明，实施例中所用的技术手段为本领域技术人员所熟知的常规手段。除非特别说明，本发明采用的试剂、方法和设备为本技术领域常规试剂、方法和设备。
实施例1
1.称取90gα-Si3N4粉体、5gAl2O3和5gY2O3粉体，将所有粉体与无水乙醇球磨混合球磨24h，将混合粉体烘干，装入直径30mm的柱状石墨模具中压实，采用放电等离子烧结设备以150℃/min的升温速率升温，升至1200℃开始充氮气并且开始加压，继续将温度升至1650℃，同时压力升至30MPa；升温程序执行完毕后保温保压5min；然后按照以下降温程序进行：以100℃/min的降温速率降温，同时进行泄压，降至1200℃泄压完毕，温度降至850℃随炉降温。冷却后取出脱模，获得柱状的Si3N4陶瓷预烧结体；
2.称取88.3gα-Si3N4粉体、2.9gAl2O3、4.7AlN和4.1gY2O3粉体，将所有粉体与无水乙醇球磨混合球磨24h，将混合粉体烘干，装入内径40mm，外径60mm的环状石墨模具中压实，采用放电等离子烧结设备以150℃/min的升温速率升温，升至1200℃开始充氮气并且开始加压，继续将温度升至1650℃，同时压力升至30MPa；升温程序执行完毕后保温保压5min；然后按照以下降温程序进行：以100℃/min的降温速率降温，同时进行泄压，降至1200℃泄压完毕，温度降至850℃随炉降温。冷却后取出脱模，获得环状的SiAlON陶瓷预烧结体。
3.将柱状的Si3N4陶瓷预烧结体置于直径60mm的圆柱状石墨模具中心位置，将环状的SiAlON陶瓷预烧结体与柱状的Si3N4陶瓷预烧结体同心放置到模具中，先在5MPa压力下以150℃/min的速率升温到1400℃，然后逐渐增加压力，以同样的速率升温到1800℃，同时加压达到30MPa，并保压保温10min，随后以速率为150℃/min降温，整个过程的保护气氛为N2，冷却后取出，脱模获得织构化的梯度陶瓷复合材料。该织构化的梯度陶瓷复合材料是由以***为环状、向心织构的SiAlON陶瓷材料和内部为柱状、随机织构的Si3N4陶瓷材料复合而成。
本实施例制得的织构化的梯度陶瓷复合材料的相对密度达到99％，***环状的SiAlON陶瓷的力学性能与物理性能在不同方向上表现出各向异性，在垂直SiAlON棒状晶粒的方向上具有最高的硬度、断裂韧性、抗弯强度，分别为18.41GPa、6.30MPa·m1/2、13.98MPa；在平行SiAlON棒状晶粒的方向上具有最高的热导率，为82W/(m.K)。内部柱状Si3N4陶瓷的力学性能与物理性能在不同方向上表现出各向异性，在垂直Si3N4棒状晶粒的方向上具有最高的硬度、断裂韧性和抗弯强度，分别为17.44GPa、7.01MPa·m1/2、13.50MPa，在平行Si3N4棒状晶粒的方向上具有最高的热导率，为95W/(m.K)。
实施例2
1.称取90gα-Si3N4粉体、5gAl2O3和5gY2O3粉体，将所有粉体与无水乙醇球磨混合球磨24h，将混合粉体烘干，装入直径30mm的柱状石墨模具中压实，采用热压烧结设备以10/min的升温速率升温，升至1000℃开始充氮气并且开始加压，继续以8℃/min的升温速率升温，将温度升至1650℃，同时压力升至30MPa；升温程序执行完毕后保温保压5min；然后按照以下降温程序进行：以10℃/min的降温速率降温，同时进行泄压，1000℃泄压完毕，温度降至850℃随炉降温。冷却后取出脱模，获得柱状的Si3N4陶瓷预烧结体；
2.称取88.3gα-Si3N4粉体、2.9gAl2O3、4.7AlN和4.1gY2O3粉体，将所有粉体与无水乙醇球磨混合球磨24h，将混合粉体烘干，装入内径40mm，外径60mm的环状石墨模具中压实，采用热压烧结设备以10/min的升温速率升温，升至1000℃开始充氮气并且开始加压，继续以8℃/min的升温速率升温，将温度升至1650℃，同时压力升至30MPa；升温程序执行完毕后保温保压5min；然后按照以下降温程序进行：以10℃/min的降温速率降温，同时进行泄压，1000℃泄压完毕，温度降至850℃随炉降温。冷却后取出脱模，获得环状的SiAlON陶瓷预烧结体。
3.将柱状的Si3N4陶瓷预烧结体置于直径60mm的圆柱状石墨模具中心位置，将环状的SiAlON陶瓷预烧结体与柱状的Si3N4陶瓷预烧结体同心放置到模具中，先在5MPa压力下以150℃/min的速率升温到1400℃，然后逐渐增加压力，以同样的速率升温到1800℃，同时加压达到30MPa，并保压保温10min，随后以速率为150℃/min降温，整个过程的保护气氛为N2，冷却后取出，脱模获得织构化的梯度陶瓷复合材料。该织构化的梯度陶瓷复合材料是由以***为环状、向心织构的SiAlON陶瓷材料和内部为柱状、随机织构的Si3N4陶瓷材料复合而成。
本实施例制得的织构化的梯度陶瓷复合材料的相对密度达到98％，***环状的SiAlON陶瓷的力学性能与物理性能在不同方向上表现出各向异性，在垂直SiAlON棒状晶粒的方向上具有最高的硬度、断裂韧性、抗弯强度，分别为18.31GPa、6.50MPa·m1/2、12.52MPa；在平行SiAlON棒状晶粒的方向上具有最高的热导率，为76W/(m.K)。内部柱状Si3N4陶瓷的力学性能与物理性能在不同方向上表现出各向异性，在垂直Si3N4棒状晶粒的方向上具有最高的硬度、断裂韧性和抗弯强度，分别为17.82GPa、7.34MPa·m1/2、13.09MPa，在平行Si3N4棒状晶粒的方向上具有最高的热导率，为93W/(m.K)。
图1是本发明的陶瓷预烧结体在模具内的位置及陶瓷材料的织构方式。其中，1为模具；2为环状的陶瓷预烧结体；3为柱状的陶瓷预烧结体3。箭头方向代表着陶瓷材料的织构方向，从图1中可知，***的环状预烧结体发生向心织构，内部的柱状预烧结体发生随机织构。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合和简化，均应为等效的置换方式，都包含在本发明的保护范围之内。

Claims (7)

1.一种织构化的梯度陶瓷复合材料，其特征在于，所述织构化的梯度陶瓷复合材料由***为环状、向心织构的SiAlON陶瓷和内部为柱状、随机织构的Si3N4陶瓷组成，是将柱状的Si3N4陶瓷预烧结体置于环状的SiAlON陶瓷预烧结体中，在1750~1800℃，同时加压30~40MPa，通过放电等离子烧结制得；在烧结过程中陶瓷预烧结体受到机械压力分别向外向内流动，填充中间的空位，直至二者完全烧结到一起；
所述的织构化的梯度陶瓷复合材料的制备方法，具体步骤包括：
S1. 将α-Si3N4、Y2O3、Al2O3和AlN粉体混合干燥后，置于石墨模具中，通过热压烧结或放电等离子烧结，升温至1450~1650℃，烧结压力为25~35MPa，保护气氛为N2，冷却后取出脱模，制得环状的SiAlON陶瓷预烧结体；
S2. 将α-Si3N4、Y2O3和Al2O3粉体混合干燥后，置于石墨模具中，通过热压烧结或放电等离子烧结，升温至1450~1650℃，烧结压力为25~35MPa，保护气氛为N2，冷却后取出脱模，制得柱状的Si3N4陶瓷预烧结体；
S3. 将环状的SiAlON陶瓷预烧结体和柱状的Si3N4陶瓷预烧结体置于同一柱状模具中，柱状的Si3N4陶瓷预烧结体置于环状的SiAlON陶瓷预烧结体内，二者中间留有空位，通过放电等离子烧结，先在3~5MPa压力下以130~150℃/min的速率升温，升至1000~1200℃时开始充氮气并且逐渐增加压力，以同样的速率升温至1750~1800℃，同时加压达到30~40MPa，并保压保温8~10min，随后以130~150℃/min的速率降温，冷却后取出，制得织构化的梯度陶瓷复合材料。
2.根据权利要求1所述的织构化的梯度陶瓷复合材料，其特征在于，步骤S1中，按照α-Si3N4粉体的总质量为100%计算，Al2O3的质量百分比为2~5%，AlN的质量百分比为5~8%，Y2O3的质量百分比为3~5%。
3.根据权利要求1所述的织构化的梯度陶瓷复合材料，其特征在于，步骤S2中，按照α-Si3N4粉体的总质量为100%计算，Al2O3的质量百分比为5~10%，Y2O3的质量百分比为5~10%。
4.权利要求1-3任一项所述的织构化的梯度陶瓷复合材料的制备方法，其特征在于，包括以下步骤：
S1. 将α-Si3N4、Y2O3、Al2O3和AlN粉体混合干燥后，置于石墨模具中，通过热压烧结或放电等离子烧结，升温至1450~1650℃，烧结压力为25~35MPa，保护气氛为N2，冷却后取出脱模，制得环状的SiAlON陶瓷预烧结体；
S2. 将α-Si3N4、Y2O3和Al2O3粉体混合干燥后，置于石墨模具中，通过热压烧结或放电等离子烧结，升温至1450~1650℃，烧结压力为25~35MPa，保护气氛为N2，冷却后取出脱模，制得柱状的Si3N4陶瓷预烧结体；
S3. 将环状的SiAlON陶瓷预烧结体和柱状的Si3N4陶瓷预烧结体置于同一柱状模具中，柱状的Si3N4陶瓷预烧结体置于环状的SiAlON陶瓷预烧结体内，二者中间留有空位，通过放电等离子烧结，先在3~5MPa压力下以130~150℃/min的速率升温，升至1000~1200℃时开始充氮气并且逐渐增加压力，以同样的速率升温至1750~1800℃，同时加压达到30~40MPa，并保压保温8~10min，随后以130~150℃/min的速率降温，冷却后取出，制得织构化的梯度陶瓷复合材料。
5.根据权利要求4所述的织构化的梯度陶瓷复合材料的制备方法，其特征在于，步骤S1和S2中所述热压烧结的程序为：以10~14℃/min的速率升温至800~1000℃开始充氮气并且开始加压，继续以6~8℃/min的速率升温至1450~1650℃，同时压力升至25~35MPa；升温程序执行完毕后保温保压3~7min；再以10~12℃/min的速率降温至1000~1200℃泄压完毕，降温至750~850℃随炉降温；所述放电等离子烧结的程序为：以130~150℃/min的速率升温至1000~1200℃时开始充氮气并且开始加压，继续将温度升至1450~1650℃，同时压力升至25~35MPa；升温程序执行完毕后保温保压3~7min；然后以80~100℃/min的速率降温至1000~1200℃泄压完毕，降温至750~850℃随炉降温。
6.根据权利要求4所述的织构化的梯度陶瓷复合材料的制备方法，其特征在于，步骤S1和S2中所述α-Si3N4的纯度均为95~100%，粒径为<0.2μm；所述Al2O3的纯度为99.9~100%，粒径为<0.2μm；所述AlN的纯度为99.9~100%，粒径为3~5μm；所述Y2O3的纯度为99.9~100%，粒径为3~6μm。
7.权利要求1-3任一项所述的织构化的梯度陶瓷复合材料在切削难加工材料、航空航天耐磨零部件或轴承制备领域中的应用。
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