CN105152655A - 一种陶瓷的织构化方法 - Google Patents

一种陶瓷的织构化方法 Download PDF

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CN105152655A
CN105152655A CN201510414902.4A CN201510414902A CN105152655A CN 105152655 A CN105152655 A CN 105152655A CN 201510414902 A CN201510414902 A CN 201510414902A CN 105152655 A CN105152655 A CN 105152655A
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texturing
powder
silicon nitride
texturing method
ceramic
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CN105152655B (zh
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伍尚华
蒋强国
郭伟明
古尚贤
周茂鹏
刘伟
程利霞
王成勇
王启民
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Guangdong University of Technology
Dongguan South China Design and Innovation Institute
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Guangdong University of Technology
Dongguan South China Design and Innovation Institute
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Abstract

本发明提供一种陶瓷的织构化方法，包括步骤：a、配料，将含有烧结助剂的氮化硅粉体混匀，干燥；b、成型；将干燥后的粉体经过钢模干压和冷等静压制得一定形状的坯体；c、织构化，采用热压流动烧结的方法使步骤b制得的坯体在一维或二维方向流动从而实现晶粒定向排布和异向生长，制得高性能陶瓷；其中热压力为10-50MPa，温度为1000-2000℃。本发明通过热压流动烧结法，使烧结材料具有一定的流动充型性能，可用于在高温时的复杂形状的成型，并且伴有相应方向上的织构化。

Description

一种陶瓷的织构化方法
技术领域
本发明属于陶瓷材料技术领域，特别涉及一种陶瓷的织构化方法。
背景技术
结构陶瓷以其高硬度、低密度、高强、耐腐蚀、耐高温性能好等诸多优点，被广泛研究和应用，主要应用在高温、腐蚀、强磨损等极端环境和一些电子元器件上，例如陶瓷发动机涡轮、铸铝坩埚、刀具、轴承球、散热基板等。但是，陶瓷材料的脆性、热学性能极大的限制了其在个领域中的应用。近几十年的研究，通过织构化的方法有效提高了其力学、热学等性能。主要方法有模板晶粒法、热加工法、磁场法、电场法等。模板晶粒法工艺过程繁复，织构化程度低；热加工法高耗能并且织构化程度不高；磁场法和电场法，对设备要求极高，成本高，极大限制了实际应用。为此，如何开发一种陶瓷的织构化方法，能够提高织构化程度并且能耗低对设备要求不高，是目前领域内难以克服的问题。
发明内容
针对以上问题，本发明的目的是一种新的陶瓷的织构化方法—热压流动烧结法，可以完成对氮化硅陶瓷材料的一维、二维织构化，同时利用烧结样品的变形量控制织构化程度，赋予材料在不同方向上特殊的力学、热学性能和耐磨性等。
为实现以上目的，本发明的技术方案为：
一种陶瓷的织构化方法，包括步骤：a、配料，将含有烧结助剂的氮化硅粉体混匀，干燥；b、成型；将干燥后的粉体经过钢模干压和冷等静压制得一定形状的坯体；c、织构化，采用热压流动烧结的方法使步骤b制得的坯体在一维或二维方向流动从而实现晶粒定向排布和异向生长，制得高性能陶瓷；其中热压力为10-50MPa，温度为1000-2000℃。
所述烧结助剂为碱金属氧化物或稀土金属氧化物的任一种或多种。
所述步骤a的配料包括混料和干燥两个步骤，混料为将烧结助剂和陶瓷粉体加入溶剂中，配置成浆料，然后加入氮化硅研磨球进行球磨，氮化硅研磨球和粉体的重量比为1-5：1，并进行超声分散，氮化硅研磨球和混合粉体的重量比为1-5：1；其中烧结助剂和α相氮化硅粉体的重量比为0.5-35:100。
所述溶剂为水、无水乙醇、丙酮、丙醇的任一种或多种，混合粉体和溶剂的体积比为1：1-3。
将步骤混料制得的浆料放入旋转蒸发仪，加热温度为40-60℃，粉体干燥后过筛。
所述粉体干燥后过筛所用为30-200目筛。
所述步骤b成型包括粉料在钢模内干压成型后，再经过冷等静压成型两个步骤。
所述冷等静压的压力为50-300MPa。
所述织构化过程在石墨模具内进行，织构化步骤中采用流动的惰性气体为保护气氛。
一种陶瓷，由本发明的陶瓷的织构化方法所制得，用于制造金属切削刀具、散热基板、轴承球、铸铝坩埚、陶瓷发动机涡轮及其他结构件。
本发明的有益效果是：
1、本发明通过热压流动烧结，在烧结初期就能完成织构化，提高织构化程度；进一步提高氮化硅陶瓷的韧性、强度和导热性。通过本发明方法制备的氮化硅陶瓷的韧性可高达14MPa·m1/2，抗弯强度高达1800MPa，热导率高达150W·m-1·K-1，可应用于氮化硅陶瓷刀具、轴承球、散热基板/电路板或其它耐磨耐高温的关键零部件。
2、通过热压流动烧结法，使烧结材料具有一定的流动充型性能，可用于在高温时的复杂形状的成型，并且伴有相应方向上的织构化。
3、利用坯体一维或二维方向上的热压形变量控制织构化程度，氮化硅的织构化率可以从无织构化到完全织构化。
4、通过热压流动的方法，坯体在模具中一维或二维方向上流动，使晶粒定向排布，并促进晶粒的异向生长。
附图说明
图1为实施例1织构化前后的模具剖面图，A为步骤c织构化前的模具剖面图；B为步骤c织构化后的模具剖面图；
图2为实施例1氮化硅陶瓷二维织构化的原理图；
图3为二维织构化氮化硅陶瓷经等离子蚀刻后的微观结构图，其中a为垂直于热压方向的氮化硅等离子蚀刻后的微观结构图，b为平行于于热压方向的氮化硅等离子蚀刻后的微观结构图；
图4为实施例4织构化前后的模具剖面图，左边是图A，为步骤c织构化前的模具剖面图；右边是图B，为步骤c织构化后的模具剖面图。
图中：1、石墨模具；2、上冲头；3、下冲头；4、坯体；5、压力；6、陶瓷。
具体实施方式
根据附图进一步说明本发明的一种实施方式。
实施例1：参考图1、图2和图3，
为了更充分理解本发明的技术内容，下面结合具体实施例对本发明的技术方案作进一步介绍和说明。
实施例1-4的氮化硅陶瓷的制备方法如下：
实施例1：
Si3N4-MgO-Yb2O3-La2O3
a1、混料：将2.8克MgO、5.56克Yb2O3和5.56克La2O3加入无水乙醇中，配成混合粉体，超声分散10分钟，放入高纯氮化硅研磨球，球料比为3:1，球磨2小时，再加入126克α相氮化硅粉体，超声分散10分钟，再球磨12小时。
a2、干燥：将球磨后的浆料放入旋转蒸发仪，加热温度为60℃，粉体干燥后，过60目筛子。
b、成型：将干燥后的粉料利用直径50mm的钢模干压成型，压力为30MPa，获得相应形状的块体，再经过冷等静压成型为坯体，压力为200MPa。
c、织构化/烧结：用热压烧结使步骤3的坯体致密化，石墨模具直径为100mm，烧结温度到1500℃，开始加压至30MPa，在1800℃烧结，保温1小时，烧结压力为30MPa，保护气氛为流动氮气。
实施例2：
Si3N4-MgO-Yb2O3-La2O3
a1、混料：将2.8克MgO、5.56克Yb2O3和5.56克La2O3加入无水乙醇中，配成混合粉体，超声分散10分钟，放入高纯氮化硅研磨球，球料比为3:1，球磨2小时，再加入126克α相氮化硅粉体，超声分散10分钟，再球磨12小时。
a2、干燥：将球磨后的浆料放入旋转蒸发仪，加热温度为60℃，粉体干燥后，过60目筛子。
c、成型：将干燥后的粉料利用直径80mm的钢模干压成型，压力为30MPa，获得相应形状的块体，再经过冷等静压成型为坯体，压力为200MPa。
d、织构化/烧结：用热压烧结使步骤3的坯体致密化，石墨模具直径为100mm，烧结温度到1500℃，开始加压至30MPa，在1800℃烧结，保温1小时，烧结压力为30MPa，保护气氛为流动氮气。
实施例3：
Si3N4-MgO-Yb2O3-La2O3
a1、混料：将2.8克MgO、5.56克Yb2O3和5.56克La2O3加入无水乙醇中，配成混合粉体，超声分散10分钟，放入高纯氮化硅研磨球，球料比为3:1，球磨2小时，再加入126克α相氮化硅粉体，超声分散10分钟，再球磨12小时。
a2、干燥：将球磨后的浆料放入旋转蒸发仪，加热温度为60℃，粉体干燥后，过60目筛子。
b、成型：将干燥后的粉料利用直径100mm的钢模干压成型，压力为30MPa，获得相应形状的块体，再经过冷等静压成型为坯体，压力为200MPa。
c、织构化/烧结：用热压烧结使步骤3的坯体致密化，石墨模具直径为100mm，烧结温度为1800℃，保温1小时，烧结压力为30MPa，保护气氛为流动氮气。
实施例4：参考图4：
Si3N4-MgO-Yb2O3-La2O3
a1、混料：将2.8克MgO、5.56克Yb2O3和5.56克La2O3加入无水乙醇中，配成混合粉体，超声分散10分钟，放入高纯氮化硅研磨球，球料比为3:1，球磨2小时，再加入126克α相氮化硅粉体，超声分散10分钟，再球磨12小时。
a2、干燥：将球磨后的浆料放入旋转蒸发仪，加热温度为60℃，粉体干燥后，过60目筛子。
b、成型：将干燥后的粉料利用50*50mm的方钢模干压成型，压力为30MPa，获得相应形状的块体，再经过冷等静压成型为坯体，压力为200MPa。
c、织构化/烧结：用热压烧结使步骤3的坯体致密化，方形石墨模具尺寸为50*100mm，烧结温度到1500℃，开始加压至30MPa，在1800℃烧结，保温1小时，烧结压力为30MPa，保护气氛为流动氮气。
本发明陶瓷的织构化方法重要步骤c具体操作：将冷等静压后的坯体放入石墨模具内，加热至1100-1800℃，然后在上冲头和下冲头的作用下加压，坯体上的晶粒发生定向排布并且部分晶粒异向生长，得到所需的高性能陶瓷。
用金刚石工具分别对实施例1-4所制得的氮化硅陶瓷进行加工，用各实施例的氮化硅陶瓷分别制成多根3mm×4mm×45mm的样条。由实施例1的氮化硅陶瓷制成的样条记为1号样条，由实施例2-4的氮化硅陶瓷制成的样条相应地记为2-4号样条。1-4号样条用于测试氮化硅陶瓷的性能。
实施例1-4制备的氮化硅陶瓷（1-4号样条）进行如下性能测试：（a）抗弯强度与断裂韧性：每号样条中的10根用于测试氮化硅的抗弯强度，根据ASTM-C1161-02标准，四点抗弯，外跨距40mm，内跨距20mm；5根用单边桥切口法测试断裂韧性，三点抗弯，跨距为40mm，切口尺寸为150±2um。（b）热导率测试方法：利用激光导热仪测试热扩散系数，根据ASTM-E-461-01标准。（c）织构化率测试方法—利用不同面的XRD强度计算Lotgering指数。
表1实施例1-4制备的氮化硅陶瓷的性能测试结果
由表1的测试结果可知，氮化硅陶瓷经一维或者二维织构化后，较未织构化的样品，在一定方向上力学、热学性能均有很大提高。
以上所述仅以实施例来进一步说明本发明的技术内容，以便于读者更容易理解，但不代表本发明的实施方式仅限于此，任何依本发明所做的技术延伸或再创造，均受本发明的保护。

Claims (10)

1.一种陶瓷的织构化方法，包括步骤：a、配料，将含有烧结助剂的氮化硅粉体混匀，干燥；b、成型；将干燥后的粉体经过钢模干压和冷等静压制得一定形状的坯体；c、织构化，采用热压流动烧结的方法使步骤b制得的坯体在一维或二维方向流动从而实现晶粒定向排布和异向生长，制得高性能陶瓷；其中热压力为10-50MPa，温度为1000-2000℃。
2.根据权利要求1所述的陶瓷的织构化方法，所述烧结助剂为碱金属氧化物或稀土金属氧化物的任一种或多种。
3.根据权利要求1所述的陶瓷的织构化方法，所述步骤a的配料包括混料和干燥两个步骤，混料为将烧结助剂和陶瓷粉体加入溶剂中，配置成浆料，然后加入氮化硅研磨球进行球磨，氮化硅研磨球和粉体的重量比为1-5：1，并进行超声分散，氮化硅研磨球和混合粉体的重量比为1-5：1；其中烧结助剂和α相氮化硅粉体的重量比为0.5-35:100。
4.根据权利要求3所述的陶瓷的织构化方法，所述溶剂为水、无水乙醇、丙酮、丙醇的任一种或多种，混合粉体和溶剂的体积比为1：1-3。
5.根据权利要求3所述的陶瓷的织构化方法，将步骤混料制得的浆料放入旋转蒸发仪，加热温度为40-60℃，粉体干燥后过筛。
6.根据权利要求5所述的陶瓷的织构化方法，所述粉体干燥后过筛所用为30-200目筛。
7.根据权利要求5述的陶瓷的织构化方法，所述步骤b成型包括粉料在钢模内干压成型后，再经过冷等静压成型两个步骤。
8.根据权利要求7所述的陶瓷的织构化方法，所述冷等静压的压力为50-300MPa。
9.根据权利要求1所述的陶瓷的织构化方法，所述织构化过程在石墨模具内进行，织构化步骤中采用流动的惰性气体为保护气氛。
10.一种陶瓷，由权利要求1-9任一项织构化方法所制得，用于制造金属切削刀具、散热基板、轴承球、铸铝坩埚、陶瓷发动机涡轮及其他结构件。
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Address after: 523000 room 318, building 9, No. 1, Xuefu Road, Songshanhu Park, Dongguan City, Guangdong Province

Patentee after: DONGGUAN SOUTH CHINA DESIGN INNOVATION INSTITUTE

Country or region after: China

Patentee after: GUANGDONG University OF TECHNOLOGY

Address before: Building 13, No.1 Xinzhu Road Headquarters, Songshan Lake Science and Technology Industrial Park, Dongguan City, Guangdong Province, 523000

Patentee before: DONGGUAN SOUTH CHINA DESIGN INNOVATION INSTITUTE

Country or region before: China

Patentee before: GUANGDONG University OF TECHNOLOGY