CN113149663A - 一种高断裂韧性Sialon陶瓷及其制备方法和应用 - Google Patents

一种高断裂韧性Sialon陶瓷及其制备方法和应用 Download PDF

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CN113149663A
CN113149663A CN202110384589.XA CN202110384589A CN113149663A CN 113149663 A CN113149663 A CN 113149663A CN 202110384589 A CN202110384589 A CN 202110384589A CN 113149663 A CN113149663 A CN 113149663A
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sialon
powder
ceramic
fracture toughness
beta
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郭伟明
张展
谭大旺
林华泰
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Guangdong University of Technology
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Abstract

本发明属于陶瓷材料技术领域，公开了一种高断裂韧性Sialon陶瓷及其制备方法和应用。该Sialon陶瓷的主晶相为α‑Sialon或者α‑Sialon和β‑Sialon的复合相。其制备包括如下步骤：异丙醇、聚乙二醇和粉体混合，经搅拌、球磨、喷雾造粒后，得到Sialon‑Ti造粒球；再将Sialon‑Ti造粒球在真空条件升温至550～650℃脱脂，压块获得生胚；生胚在氮气气氛下置于无压炉中于1200℃进行预烧，使生胚充分氮化，然后随炉冷却；得到的预烧体在氮气气氛下进行烧结保温，烧结方式为气压烧结再随炉冷却得到Sialon陶瓷。

Description

一种高断裂韧性Sialon陶瓷及其制备方法和应用
技术领域
本发明属于陶瓷材料技术领域，特别涉及一种高断裂韧性Sialon陶瓷及其制备方法和应用。
背景技术
在现代切削加工中，陶瓷材料以其优异的耐热性、耐磨性和化学稳定性成为目前最有前途的刀具材料之一，在高速切削领域和切削难加工材料方面扮演着越来越重要的角色。Sialon陶瓷作为一种重要的Si基陶瓷，在切削高温合金(特别是镍基高温合金)的过程中发挥着重要的作用。
然而，Sialon陶瓷也具有陶瓷材料的普遍问题，α-Sialon陶瓷本身居然较高的硬度，但是本身等轴状晶粒导致了高脆性，低韧性，极大的限制了在陶瓷刀具方面的应用；β-Sialon因为长棒状晶粒的存在，极大的改善了Sialon陶瓷的断裂韧性，但也导致了较低的硬度，在陶瓷刀具应用中极大的加大了磨损消耗，降低了刀具的使用寿命。
发明内容
为了克服现有技术中存在的缺点和不足，本发明的首要目的在于提供一种高断裂韧性Sialon陶瓷的制备方法；这是一种引入金属Ti粉和晶种，经过两步烧结法完成的方法。
本发明的另一个目的在于提供一种上述制备方法制备得到的高断裂韧性Sialon陶瓷。该Sialon陶瓷的主晶相为α-Sialon或者α-Sialon和β-Sialon的复合相。
本发明的再一目的在于提供一种上述高断裂韧性Sialon陶瓷的应用。
本发明的目的通过下述技术方案实现：
一种高断裂韧性Sialon陶瓷，所述Sialon陶瓷是由以下按质量百分比计的原料制备而成：Si3N4粉体60～80wt.％、AlN粉体5～10wt.％、Al2O3粉体0～5wt.％、Ti粉体5～20wt.％、β-Sialon晶种2～10wt.％、Me2O3粉体2～15wt.％；所述β-Sialon晶种长径比为3.0-5.0，直径为0.30-0.60μm；所述Me为Mg、Ca、Y或Yb。
所述Sialon陶瓷的相对密度为95～100％，断裂韧性为6～10MPa·m1/2，维氏硬度为16～20GPa，抗弯强度为600～1000MPa。
所述Si3N4粉体的纯度为95～100％，粒径<10μm。
所述AlN粉体、A2O3粉体、Ti粉体、Me2O3粉体的纯度为99.9％。
所述β-Sialon晶种的长径比为4.5，直径为0.52μm。
所述β-Sialon晶种是由碳热还原法制备而成，具体按照以下步骤：
(1)将摩尔比为1：1：9的无水氯化铝、正硅酸乙酯和二氯甲烷混合得到反应液，置于温度>120℃的高温烘箱中中加热24h使其发生非水解溶胶-凝胶反应，然后将反应产物在温度<100℃的烘箱中干燥12h，最后在400℃进行煅烧1h，得到硅-铝混合物的前驱体；
(2)将步骤(1)所得前驱体与石墨按照1：4的质量比混合，加入4wt.％的矿化剂MgO，再加入酒精混合后球磨5h，旋蒸，在100℃烘箱中干燥24h；
(3)在N2气氛管式炉中，以5℃/min的升温速率和80ml/min的N2流量下加热到1350℃发生碳热还原反应和氮化反应8h后，于800℃热处理1h进行排碳，得到β-Sialon粉体；
(4)将β-Sialon粉体充分碾碎后过筛，得到长径比为β-Sialon晶种。
上述高断裂韧性Sialon陶瓷的制备方法，包括以下操作步骤：
(1)将Si3N4粉体、AlN粉体、Al2O3粉体、β-Sialon晶种、Ti粉体、Me2O3粉体进行混料，加入聚乙二醇作为粘结剂，经搅拌、球磨、喷雾造粒，得到Sialon-Ti造粒球；
(2)将Sialon-Ti造粒球在真空条件下升温至550～650℃脱脂并保温1～2h，升温速率为1～5℃/min，再将Sialon-Ti造粒球经压制成型，获得生胚；生胚在氮气气氛下置于无压炉中于1200℃进行预烧，使生胚充分氮化，然后随炉冷却；得到的预烧体在氮气气氛下进行高温烧结，烧结方式为气压烧结，随炉冷却得到高断裂韧性Sialon陶瓷。
步骤(2)所述高温烧结是将预烧体放入BN粉体埋床的石墨模具中，在氮气压为5～10MPa的条件下，以10℃/min的升温速率升至1700～1900℃，并保温2～4h，随后按照5～12℃/min速率降温至1200℃，再随炉冷却。
步骤(1)所述混料用溶剂为异丙醇，所述混料的时间为12～24h。
上述的一种高断裂韧性Sialon陶瓷在陶瓷领域中的应用。
本发明通过引入β-Sialon晶种添加长棒状晶粒的占比可以改善Sialon-Ti陶瓷的韧性，增加Ti金属粉体作为第二相构成既可以改善Sialon-Ti陶瓷的力学性能，又能促进其致密化。采用喷雾造粒技术对Sialon-Ti粉体进行造粒，使Ti粉体分部均匀，不会产生聚集现象。在Sialon陶瓷长棒状晶粒周围分部有均匀的经氮化处理后的Ti元素，那么在断裂过程中会出现裂纹偏转效应，可以显著提高Sialon-Ti陶瓷的断裂韧性。
本发明相对于现有技术具有如下的优点及效果：
(1)本发明通过对Sialon-Ti造粒，经过烧结后可以得到Ti元素分布均匀的Sialon陶瓷，且经过高温氮化后，降低了粉体中的氧含量，有效的提高了Sialon陶瓷的致密度和力学性能。
(2)烧结过程中引入β-Sialon晶种，极大的促使Sialon晶粒成长为长棒状，使Sialon陶瓷的断裂性能大幅度提高。
附图说明
图1为实施例1中合成Sialon-Ti陶瓷的断面图。
具体实施方式
下面结合实施例及附图对本发明作进一步详细的描述，但本发明的实施方式不限于此。
以下实施例所用的β-Sialon晶种是由碳热还原法制备而成，具体按照以下步骤：
(1)将摩尔比为1：1：9的无水氯化铝、正硅酸乙酯和二氯甲烷混合得到反应液，置于温度>120℃的高温烘箱中中加热24h使其发生非水解溶胶-凝胶反应，然后将反应产物在温度<100℃的烘箱中干燥12h，最后在400℃进行煅烧1h，得到硅-铝混合物的前驱体；
(2)将步骤(1)所得前驱体与石墨按照1：4的质量比混合，加入4wt.％的矿化剂MgO，再加入酒精混合后球磨5h，旋蒸，在100℃烘箱中干燥24h；
(3)在N2气氛管式炉中，以5℃/min的升温速率和80ml/min的N2流量下加热到1350℃发生碳热还原反应和氮化反应8h后，于800℃热处理1h进行排碳，得到β-Sialon粉体；
(4)将β-Sialon粉体充分碾碎后过筛，得到长径比为4.5，直径为0.52μm的β-Sialon晶种。
以下实施例中所用的Si3N4粉体的纯度为95～100％，粒径<10μm；所用的AlN粉体、A2O3粉体、Ti粉体、Me2O3粉体的纯度为99.9％。
实施例1
本发明高断裂韧性Sialon陶瓷，是由以下按质量百分比计的原料制备而成：Si3N4粉体75wt.％、AlN粉体10wt.％、Al2O3粉体1wt.％、Ti粉体5wt.％、β-Sialon晶种4wt.％、Me2O3粉体5wt.％；所述Me为Y。
上述高断裂韧性Sialon陶瓷按照以下方法制备而成：
(1)将Si3N4粉体、AlN粉体、Al2O3粉体、β-Sialon晶种、Ti粉体、Me2O3粉体进行混料，加入聚乙二醇作为粘结剂，以异丙醇为溶剂，搅拌，以Si3N4球为球磨介质，在行星式球磨机上混合球磨24h，喷雾造粒，得到Sialon-Ti造粒球；
(2)将Sialon-Ti造粒球在真空条件下升温至600℃脱脂并保温1h，升温速率为2℃/min，再将Sialon-Ti造粒球经压制成型，获得生坯；生胚在氮气气氛下置于无压炉中，以5℃/min的升温速率升温至1200℃，进行预烧，使生胚充分氮化，然后随炉冷却；得到的预烧体放入BN粉体埋床的石墨模具中，在氮气气氛下，以10℃/min的升温速率升至1800℃，并保温4h，(升温至1500℃开始加压3MPa，保温之前加压到8MPa)，保温结束后泄压，随后按照10℃/min速率降温至1200℃，充分氮化，再随炉冷却得到高断裂韧性Sialon陶瓷。
本实施例中制备得到的Sialon-Ti陶瓷的相对密度达到99.5％，主相为(α+β)-Sialon复合相，其断面的显微结构为图1所示。维氏硬度为18.4GPa,利用压痕法测量的断裂韧性为9.65Mpa·m1/2,维氏硬度为17.5GPa三点抗弯强度为823Mpa。
实施例2
本发明高断裂韧性Sialon陶瓷，是由以下按质量百分比计的原料制备而成：Si3N4粉体70wt.％、AlN粉体8wt.％、Al2O3粉体5wt.％、Ti粉体10wt.％、β-Sialon晶种4wt.％、Me2O3粉体3wt.％；所述Me为Y。
按照实施例1方法制备高断裂韧性Sialon陶瓷，制备所得陶瓷的相对密度为98.5％，主相为(α+β)-Sialon复合相，维氏硬度为18.3GPa，利用压痕法测量的断裂韧性为9.3Mpa·m1/2，三点抗弯强度为782Mpa。
实施例3
本发明高断裂韧性Sialon陶瓷，是由以下按质量百分比计的原料制备而成：Si3N4粉体65wt.％、AlN粉体8wt.％、Al2O3粉体4wt.％、Ti粉体15wt.％、β-Sialon晶种4wt.％、Me2O3粉体4wt.％；所述Me为Y。
按照实施例1方法制备高断裂韧性Sialon陶瓷，制备所得陶瓷的相对密度为99.0％，主相为(α+β)-Sialon复合相，维氏硬度为18.5GPa，利用压痕法测量的断裂韧性为8.9Mpa·m1/2，三点抗弯强度为780Mpa。
实施例4
本发明高断裂韧性Sialon陶瓷，是由以下按质量百分比计的原料制备而成：Si3N4粉体70wt.％、AlN粉体3wt.％、Al2O3粉体1wt.％、Ti粉体20wt.％、β-Sialon晶种2wt.％、Me2O3粉体4wt.％；所述Me为Y。
按照实施例1方法制备高断裂韧性Sialon陶瓷，制备所得陶瓷的相对密度为99％，主相为(α+β)-Sialon符合相，维氏硬度为19.2GPa，利用压痕法测量的断裂韧性为8.5Mpa·m1/2，三点抗弯强度为750Mpa。
实施例5
本发明高断裂韧性Sialon陶瓷，是由以下按质量百分比计的原料制备而成：Si3N4粉体65wt.％、AlN粉体7wt.％、Ti粉体20wt.％、β-Sialon晶种4wt.％、Me2O3粉体4wt.％；所述Me为Y。
按照实施例1方法制备高断裂韧性Sialon陶瓷，制备所得陶瓷的相对密度为98％，主相为β-Sialon相，维氏硬度为16.7GPa，利用压痕法测量的断裂韧性为7.5Mpa·m1/2，三点抗弯强度为675Mpa。
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、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 (10)

1.一种高断裂韧性Sialon陶瓷，其特征在于：所述Sialon陶瓷是由以下按质量百分比计的原料制备而成：Si3N4粉体60～80wt.％、AlN粉体5～10wt.％、Al2O3粉体1～5wt.％、Ti粉体5～20wt.％、β-Sialon晶种2～10wt.％、Me2O3粉体2～15wt.％；所述β-Sialon晶种长径比为3.0-5.0，直径为0.30-0.60μm；所述Me为Mg、Ca、Y或Yb。
2.根据权利要求1所述的一种高断裂韧性Sialon陶瓷，其特征在于：所述Sialon陶瓷的相对密度为95～100％，断裂韧性为6～10MPa·m1/2，维氏硬度为16～20GPa，抗弯强度为600～1000MPa。
3.根据权利要求1所述的一种高断裂韧性Sialon陶瓷，其特征在于：所述Si3N4粉体的纯度为95～100％，粒径<10μm。
4.根据权利要求1所述的一种高断裂韧性Sialon陶瓷，其特征在于：所述AlN粉体、A2O3粉体、Ti粉体、Me2O3粉体的纯度为99.9％。
5.根据权利要求1所述的一种高断裂韧性Sialon陶瓷，其特征在于：所述β-Sialon晶种的长径比为4.5，直径为0.52μm。
6.根据权利要求1所述的一种高断裂韧性Sialon陶瓷，其特征在于：所述β-Sialon晶种是由碳热还原法制备而成，具体按照以下步骤：
(1)将摩尔比为1：1：9的无水氯化铝、正硅酸乙酯和二氯甲烷混合得到反应液，置于温度>120℃的高温烘箱中中加热24h使其发生非水解溶胶-凝胶反应，然后将反应产物在温度<100℃的烘箱中干燥12h，最后在400℃进行煅烧1h，得到硅-铝混合物的前驱体；
(2)将步骤(1)所得前驱体与石墨按照1：4的质量比混合，加入4wt.％的矿化剂MgO，再加入酒精混合后球磨5h，旋蒸，在100℃烘箱中干燥24h；
(3)在N2气氛管式炉中，以5℃/min的升温速率和80ml/min的N2流量下加热到1350℃发生碳热还原反应和氮化反应8h后，于800℃热处理1h进行排碳，得到β-Sialon粉体；
(4)将β-Sialon粉体充分碾碎后过筛，得到β-Sialon晶种。
7.根据权利要求1所述的一种高断裂韧性Sialon陶瓷的制备方法，其特征在于包括以下操作步骤：
(1)将Si3N4粉体、AlN粉体、Al2O3粉体、β-Sialon晶种、Ti粉体、Me2O3粉体进行混料，加入聚乙二醇作为粘结剂，经搅拌、球磨、喷雾造粒，得到Sialon-Ti造粒球；
(2)将Sialon-Ti造粒球在真空条件下升温至550～650℃脱脂并保温1～2h，升温速率为1～5℃/min，再将Sialon-Ti造粒球经压制成型，获得生胚；生胚在氮气气氛下置于无压炉中于1200℃进行预烧，使生胚充分氮化，然后随炉冷却；得到的预烧体在氮气气氛下进行高温烧结，烧结方式为气压烧结，随炉冷却得到高断裂韧性Sialon陶瓷。
8.根据权利要求7所述的制备方法，其特征在于：步骤(2)所述高温烧结是将预烧体放入BN粉体埋床的石墨模具中，在氮气压为5～10MPa的条件下，以10℃/min的升温速率升至1700～1900℃，并保温2～4h，随后按照5～12℃/min速率降温至1200℃，再随炉冷却。
9.根据权利要求7所述的制备方法，其特征在于：步骤(1)所述混料用溶剂为异丙醇，所述混料的时间为12～24h。
10.根据权利要求1所述的一种高断裂韧性Sialon陶瓷在陶瓷领域中的应用。
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