CN105601284A - 一种Sialon-Ti（CN）陶瓷材料及其制备方法 - Google Patents

一种Sialon-Ti（CN）陶瓷材料及其制备方法 Download PDF

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CN105601284A
CN105601284A CN201610066030.1A CN201610066030A CN105601284A CN 105601284 A CN105601284 A CN 105601284A CN 201610066030 A CN201610066030 A CN 201610066030A CN 105601284 A CN105601284 A CN 105601284A
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sialon
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吕志杰
杨广安
程凯强
邓莉莉
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Shandong Jianzhu University
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Abstract

本发明提供一种Sialon-Ti(CN)陶瓷材料及其制备方法，属于新材料技术领域，本发明Sialon-Ti(CN)陶瓷材料包括如下重量百分比的原料：0.5μmSi3N450％-70％，0.5μmAl2O38％-10％，40nmAlN3％-4％，50nmTi(CN)10％-30％，Y2O35％-6％。先将40nmAlN粉末和50nmTi(CN)粉末分别在无水乙醇中利用聚乙二醇分散剂进行超声搅拌分散制成悬浮液，然后将两悬浮液混合，并混入0.5μmSi3N4、0.5μmAl2O3粉末及助烧结剂Y2O3，球磨机混料，真空干燥，过筛，装入石墨模具，真空热压烧结。制备出Sialon-Ti(CN)陶瓷复合材料硬度可达HV17.8Gpa，抗弯强度可达790Mpa，断裂韧性可达8.0Mpa·m1/2。

Description

一种Sialon-Ti（CN）陶瓷材料及其制备方法
技术领域
本发明属于材料科学技术领域，特别涉及一种Sialon-Ti(CN)陶瓷材料及其制备方法。
背景技术
Sialon是存在于Si-Al-O-N和相关体系中氮化硅固溶体的总称，因其晶体构型不同而具有不同的结构和性质。由于Sialon陶瓷在高温下具有良好的机械性能、抗热震性能和良好的抗氧化性，膨胀系数小，化学稳定性高，耐腐蚀。可用做金属压延或拉丝模，也是高速粗加工铸铁和镍基合金较好的刀具材料之一。
目前商品化的Sialon刀片(牌号KY1540、CC6060)，性能参数分别为：KY1540维氏硬度为16.52GPa，韧性为6.7Mpa·m1/2；CC6060维氏硬度为15.33GPa，韧性为4.44Mpa·m1/2(涂桂朝，伍尚华，刘佳等，Sialon陶瓷刀具高速切削高温合金Inconel718的切削性能和磨损机理的研究，硅酸盐通报，2015，34(9)：2624)。为提高Sialon陶瓷材料的力学性能，更好地应用于难加工材料的切削加工，可通过强韧化措施主要包括颗粒弥散增韧、相变增韧以及纤维、晶须补强等。与传统单组份陶瓷相比，这类复合材料具有耐高温、抗腐蚀、高硬度、高强度等优点。因此，探索合理的组分配比和烧结工艺，制备出强度、韧性和硬度较高的Sialon基陶瓷材料是非常重要的。
发明内容
本发明的目的在于提供一种Sialon-Ti(CN)陶瓷材料的制备方法，使用本发明的方法制备的陶瓷复合材料具有较高的硬度、抗弯强度和断裂韧性，可用作制备陶瓷刀具。
为此，本发明采用技术方案是，一种Sialon-Ti(CN)陶瓷材料，包括如下重量百分比的原料：0.5μmSi3N450％-70％，0.5μmAl2O38％-10％，40nmAlN3％-4％，50nmTi(CN)10％-30％，Y2O35％-6％。
本发明Sialon-Ti(CN)陶瓷材料，制备方法是，先将40nmAlN粉末和50nmTi(CN)粉末分别在无水乙醇中利用聚乙二醇分散剂进行超声搅拌分散制成悬浮液，然后将两悬浮液混合，并混入0.5μmSi3N4、0.5μmAl2O3粉末及助烧结剂Y2O3，球磨机混料，真空干燥，过筛，装入石墨模具，真空热压烧结。
具体步骤如下：
(1)将40nmAlN粉末加无水乙醇配制成2vol％悬浮液，加入聚乙二醇作为分散剂，超声分散同时搅拌30分钟，并用氨水调节悬浮液pH＝9-10，得纳米AlN悬浮液；
(2)将50nmTi(CN)粉末加无水乙醇配制成2vol％悬浮液，加入聚乙二醇作为分散剂，超声分散同时搅拌30分钟，并用氨水调节悬浮液pH＝9-10，得纳米Ti(CN)悬浮液；
(3)将得到的纳米AlN悬浮液及纳米Ti(CN)悬浮液混合，并加入0.5μmSi3N4、0.5μmAl2O3及Y2O3，形成混合浆料，将混合浆料加入料筒中，在球磨机上混料球磨10-24小时，再经真空干燥，过120目筛，装瓶密封保存；
(4)将步骤(3)获得的干燥过筛后的粉体装入石墨模具，在烧结炉中采用真空热压烧结制成Sialon-Ti(CN)陶瓷材料。
所述步骤(1)所用聚乙二醇分子量为1450，添加量为AlN质量的0.25wt.％-0.3wt.％。
所述步骤(2)聚乙二醇所用聚乙二醇分子量为4000-6000，添加量为Ti(CN)质量的0.35wt.％。
所述步骤(4)真空热压烧结：在温度低于1200℃时，温升70-80℃/min，压力逐渐升至30MP，炉温大于1200℃时，温升45℃/min，直至1600-1700℃，然后保温50min，制成Sialon-Ti(CN)陶瓷材料。
Sialon，其通式为Si6-zAIzOzN8-z，式中Z为O原子置换N原子数，Z∈[O，4.2]，本发明中Z＝1，本发明所制备的陶瓷复合材料具有更高的硬度、抗弯强度和断裂韧性，用其制备的陶瓷刀具，具有更好的切削性能和更小的磨损。
本发明具有如下有益效果：
(1)本发明通过微米Si3N4粉末、微米Al2O3粉体、纳米AlN粉体和纳米Ti(CN)粉体的混合及热压烧结，充分发挥β-Sialon柱状晶粒的类晶须增韧与Ti(CN)颗粒补强增韧协同效应，制备出具有较高综合力学性能的Sialon-Ti(CN)陶瓷复合材料。
(2)采用纳米AlN与纳米Ti(CN)，可有效降低烧结温度，抑制基体晶粒异常长大，细化了材料晶粒；同时纳米级Ti(CN)晶粒分布于基体晶粒内，较大的Ti(CN)粒位于晶界处。“内晶型”结构引起的裂纹偏转和裂纹钉扎，有效提高材料的韧性。
(3)Sialon-Ti(CN)微纳米复合材料断裂方式为穿晶断裂和沿晶断裂的复合型。材料断口可观察到明显的柱状β-Sialon晶粒断裂、桥接、拔出及裂纹偏转等，提高复合材料的强度和韧性；该陶瓷复合材料的硬度HV可达17.8Gpa，抗弯强度可达790Mpa，断裂韧性可达8.0Mpa·m1/2。
附图说明
图1为本发明制备的Sialon-Ti(CN)陶瓷材料断口扫描电镜照片。
图2为本发明制备的Sialon-Ti(CN)陶瓷材料平面裂纹扩展扫描电镜照片。
具体实施方式
为阐明对本发明特征的理解，下面结合实施实例对本发明做进一步阐述。
实施例1：一种Sialon-Ti(CN)陶瓷材料，包括如下重量百分比的原料：0.5μmSi3N470％，0.5μmAl2O310％，40nmAlN4％，50nmTi(CN)11％，助烧结剂Y2O35％。
制备方法是：(1)将40nmAlN粉末加无水乙醇配制成2vol％悬浮液，加入分子量1540聚乙二醇作为分散剂，添加量为AlN粉末质量的0.25wt.％，超声分散同时搅拌30分钟，并用氨水调节悬浮液pH＝9，得纳米AlN悬浮液；
(2)将50nmTi(CN)粉末加无水乙醇配制成2vol％悬浮液，加入分子量4000的聚乙二醇作为分散剂，添加量为Ti(CN)质量的0.35wt.％，超声分散同时搅拌30分钟，并用氨水调节悬浮液pH＝9，得纳米Ti(CN)悬浮液；
(3)将得到的纳米AlN悬浮液及纳米Ti(CN)悬浮液混合，并加入0.5μmSi3N4、0.5μmAl2O3及Y2O3，形成混合浆料，将混合浆料加入料筒中，在球磨机上混料球磨10小时，再经真空干燥，过120目筛，装瓶密封保存；
(4)将步骤(3)获得的干燥过筛后的粉体装入石墨模具，在烧结炉中采用真空热压烧结：在温度低于1200℃时，温升75℃/min，压力逐渐升至30MP，炉温大于1200℃时，温升45℃/min，直至1700℃，然后保温50min，制备成Sialon-Ti(CN)陶瓷材料。
复合材料的力学性能为：维氏硬度16.5Gpa，抗弯强度690Mpa，断裂韧性7.3Mpa·m1/2，相对密度98.4％。
其中，相对密度为实际密度/理论密度，其中实际密度用排水法测试，然后再用实际密度/理论密度，得到相对密度，反映了烧结材料的致密程度。
实施例2：一种Sialon-Ti(CN)陶瓷材料，包括如下重量百分比的原料：0.5μmSi3N465％，0.5μmAl2O39％，40nmAlN4％，50nmTi(CN)16％，助烧结剂Y2O36％。
制备方法是：(1)将40nmAlN粉末加无水乙醇配制成2vol％悬浮液，加入分子量1540聚乙二醇作为分散剂，添加量为AlN粉末质量的0.3wt.％，超声分散同时搅拌30分钟，并用氨水调节悬浮液pH＝9.5，得纳米AlN悬浮液；
(2)将50nmTi(CN)粉末加无水乙醇配制成2vol％悬浮液，加入分子量6000的聚乙二醇作为分散剂，添加量为Ti(CN)质量的0.35wt.％，超声分散同时搅拌30分钟，并用氨水调节悬浮液pH＝10，得纳米Ti(CN)悬浮液；
(3)将得到的纳米AlN悬浮液及纳米Ti(CN)悬浮液混合，并加入0.5μmSi3N4、0.5μmAl2O3及Y2O3，形成混合浆料，将混合浆料加入料筒中，在球磨机上混料球磨20小时，再经真空干燥，过120目筛，装瓶密封保存；
(4)将步骤(3)获得的干燥过筛后的粉体装入石墨模具，在烧结炉中采用真空热压烧结：在温度低于1200℃时，温升80℃/min，压力逐渐升至30MP，炉温大于1200℃时，温升45℃/min，直至1650℃，然后保温50min，制备成Sialon-Ti(CN)陶瓷材料。
复合材料的力学性能为：维氏硬度HV17.8Gpa，抗弯强度790Mpa，断裂韧性8.0Mpa·m1/2，相对密度98.6％。如图1和图2所示。
实施例3：一种Sialon-Ti(CN)陶瓷材料，包括如下重量百分比的原料：0.5μmSi3N455％，0.5μmAl2O38％，40nmAlN3％，50nmTi(CN)28％，助烧结剂Y2O36％。
制备方法是：(1)将40nmAlN粉末加无水乙醇配制成2vol％悬浮液，加入分子量1540聚乙二醇作为分散剂，添加量为AlN粉末质量的0.3wt.％，超声分散同时搅拌30分钟，并用氨水调节悬浮液pH＝9.5，得纳米AlN悬浮液；
(2)将50nmTi(CN)粉末加无水乙醇配制成2vol％悬浮液，加入分子量6000的聚乙二醇作为分散剂，添加量为Ti(CN)质量的0.35wt.％，超声分散同时搅拌30分钟，并用氨水调节悬浮液pH＝10，得纳米Ti(CN)悬浮液；
(3)将得到的纳米AlN悬浮液及纳米Ti(CN)悬浮液混合，并加入0.5μmSi3N4、0.5μmAl2O3及Y2O3，形成混合浆料，将混合浆料加入料筒中，在球磨机上混料球磨10小时，再经真空干燥，过120目筛，装瓶密封保存；
(4)将步骤(3)获得的干燥过筛后的粉体装入石墨模具，在烧结炉中采用真空热压烧结：在温度低于1200℃时，温升70℃/min，压力逐渐升至30MP，炉温大于1200℃时，温升45℃/min，直至1700℃，然后保温50min，制备成Sialon-Ti(CN)陶瓷材料。
复合材料的力学性能为：维氏硬度HV18Gpa，抗弯强度670Mpa，断裂韧性6.5Mpa·m1/2，相对密度98.3％。
对比例1、用本发明实施例1-3所获得的陶瓷材料与现有商品化的Sialon刀片，牌号KY1540、CC6060，进行对比，结果如表1所示：
表1本发明实施例1-3陶瓷材料与KY1540、CC6060对比结果
维氏硬度HV 断裂韧性
实施例1 16.5Gpa 7.3Mpa·m1/2
实施例2 17.8Gpa 8.0Mpa·m1/2
实施例3 18Gpa 6.5Mpa·m1/2
对比例1(KY1540) 16.52GPa 6.7Mpa·m1/2
对比例2(CC6060) 15.33GPa 4.44Mpa·m1/2
由此可见，本发明所获得的陶瓷材料其维氏硬度较对比例高，具有更好的断裂韧性。这是因为，本发明采用的各原料及特定的制备方法，可以充分发挥β-Sialon柱状晶粒的类晶须增韧与Ti(CN)颗粒补强增韧协同效应，使材料的力学性能更好。本发明材料内纳米级Ti(CN)晶粒分布于基体晶粒内，较大的Ti(CN)粒位于晶界处，“内晶型”结构引起的裂纹偏转和裂纹钉扎，有效提高材料的韧性。且断裂方式为穿晶断裂和沿晶断裂的复合型。材料断口可观察到明显的柱状β-Sialon晶粒断裂、桥接、拔出及裂纹偏转等，共同提高复合材料的强度和韧性。
应理解，这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解，在阅读了本发明内容之后，本领域技术人员可以对本发明作各种改动或修改，这些等价形式同样落于本申请权利要求书所限定的范围。本发明未详细说明部分为本领域技术人员公知技术。

Claims (6)

1.一种Sialon-Ti(CN)陶瓷材料，其特征在于，包括如下重量百分比的原料：0.5μmSi3N450％-70％，0.5μmAl2O38％-10％，40nmAlN3％-4％，50nmTi(CN)10％-30％，Y2O35％-6％。
2.制备权利要求1所述Sialon-Ti(CN)陶瓷材料的方法，其特征是，先将40nmAlN粉末和50nmTi(CN)粉末分别在无水乙醇中利用聚乙二醇分散剂进行超声搅拌分散制成悬浮液，然后将两悬浮液混合，并混入0.5μmSi3N4、0.5μmAl2O3粉末及助烧结剂Y2O3，球磨机混料，真空干燥，过筛，装入石墨模具，真空热压烧结。
3.如权利要求2所述的制备Sialon-Ti(CN)陶瓷材料的方法，其特征是，具体步骤如下：
(1)将40nmAlN粉末加无水乙醇配制成2vol％悬浮液，加入聚乙二醇作为分散剂，超声分散同时搅拌30分钟，并用氨水调节悬浮液pH＝9-10，得纳米AlN悬浮液；
(2)将50nmTi(CN)粉末加无水乙醇配制成2vol％悬浮液，加入聚乙二醇作为分散剂，超声分散同时搅拌30分钟，并用氨水调节悬浮液pH＝9-10，得纳米Ti(CN)悬浮液；
(3)将得到的纳米AlN悬浮液及纳米Ti(CN)悬浮液混合，并加入0.5μmSi3N4、0.5μmAl2O3及Y2O3，形成混合浆料，将混合浆料加入料筒中，在球磨机上混料球磨10-24小时，再经真空干燥，过120目筛，装瓶密封保存；
(4)将步骤(3)获得的干燥过筛后的粉体装入石墨模具，在烧结炉中采用真空热压烧结制成Sialon-Ti(CN)陶瓷材料。
4.如权利要求3所述的制备Sialon-Ti(CN)陶瓷材料的方法，其特征是，所述步骤(1)所用聚乙二醇分子量为1450，添加量为AlN质量的0.25wt.％-0.3wt.％。
5.如权利要求3所述的制备Sialon-Ti(CN)陶瓷材料的方法，其特征是，所诉步骤(2)聚乙二醇所用聚乙二醇分子量为4000-6000，添加量为Ti(CN)质量的0.35wt.％。
6.如权利要求3所述的制备Sialon-Ti(CN)陶瓷材料的方法，其特征是，所述步骤(4)真空热压烧结：在温度低于1200℃时，温升70-80℃/min，压力逐渐升至30MP，炉温大于1200℃时，温升45℃/min，直至1600-1700℃，然后保温50min，制成Sialon-Ti(CN)陶瓷材料。
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