CN111517798A - 一种碳化物基陶瓷材料、制备方法及其应用 - Google Patents

一种碳化物基陶瓷材料、制备方法及其应用 Download PDF

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CN111517798A
CN111517798A CN202010355781.1A CN202010355781A CN111517798A CN 111517798 A CN111517798 A CN 111517798A CN 202010355781 A CN202010355781 A CN 202010355781A CN 111517798 A CN111517798 A CN 111517798A
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powder
carbide
ceramic material
based ceramic
temperature
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戴培赟
李晓丽
王东娟
殷铭良
路金喜
李�根
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WEIFANG SCHOOL OF ECONOMICS
WEIFANG BUSINESS VOCATIONAL COLLEGE
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WEIFANG SCHOOL OF ECONOMICS
WEIFANG BUSINESS VOCATIONAL COLLEGE
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Abstract

本发明公开了一种碳化物基陶瓷材料及其制备方法和应用，以质量份数计，原料包括：碳化硅粉、硅粉、Ti‑Si‑Fe合金粉、生物炭、粘结剂；制备方法，包括将原料混匀后置于球磨机中，加入球磨球进行球磨；所得球磨料置于喷雾造粒机中，通过控制喷雾造粒工艺参数制得造粒粉料，造粒粉料置于模具中压制成型；成型后的试样固化12‑24h后，在氮气气氛，800‑1000℃条件下保温1‑3h，然后升温至1300‑1450℃高温烧结2‑5h冷却至室温得碳化物基陶瓷材料。本发明制备的碳化物基陶瓷材料具有极好的硬度、密度及强度，可满足工业化生产的需求。

Description

一种碳化物基陶瓷材料、制备方法及其应用
技术领域
本发明属于陶瓷材料领域，具体涉及一种碳化物基陶瓷材料、制备方法及其应用。
背景技术
碳化硅陶瓷，别名金刚砂，属于一种新型无机非金属材料，其不仅具有优良的常温力学性能，如高的抗弯强度、优良的抗氧化性、良好的耐腐蚀性、高的抗磨损以及低的摩擦系数，而且高温力学性能(强度、抗蠕变性等)也是已知陶瓷材料中最佳的。碳化硅陶瓷是陶瓷材料中高温强度最好的材料，高温强度可一直维持到1600℃。此外，碳化硅陶瓷在高温环境下，表面可以生成一层致密的二氧化硅膜，从而使其抗氧化性也是所有非氧化物陶瓷中最好的。
碳化硅陶瓷作为少数几种适合用作高温结构零部件的候选材料之一，在高温、热冲击、腐蚀性等恶劣环境中显示出其独有的优越性。但由于碳元素与硅元素之间以共价键存在，非常稳定，因此其晶界能极高，在烧结过程时，需要获取大量的能量，才能形成晶界，构成碳化硅，由此影响了碳化硅的烧结效率。此外，烧结中，碳化硅易被氧化形成一层致密的氧化膜，该氧化膜抑制了碳化硅的扩散，降低了碳化硅的成型速度以及致密性，从而影响了碳化硅的烧结性能，使制得的碳化硅陶瓷密度较低，气孔率较高，无法满足工业化生产的需求。
发明内容
为解决上述技术问题，本发明提供一种碳化物基陶瓷材料、制备方法及其应用，以提高碳化硅的烧结效率，改善碳化硅的烧结性能，提高碳化硅陶瓷材料的成型速度和致密性。
本发明的技术方案之一，一种碳化物基陶瓷材料，以质量份数计，原料包括以下组分：碳化硅粉50-80份、硅粉10-18份、Ti-Si-Fe合金粉3-5份、生物炭15-20份、粘结剂8-10份。
优选的，所述碳化硅粉粒径为15-20μm，硅粉0.5-2μm，Ti-Si-Fe合金粉0.2-0.8μm。
粒径为15-20μm的碳化硅颗粒，有助于在烧结时形成均匀且细密的小孔，从而有助于提高陶瓷的机械强度，而且可以增加陶瓷结构的致密性，从而提高产品的抗氧化能力。
优选的，所述粘结剂为氧化铝和二氧化硅按照1∶(3-5)的质量比混合而成，氧化铝、二氧化硅粒径1-3μm。
在烧结过程中氧化铝和二氧化硅会连接在碳化硅的颗粒中间，包裹碳化硅颗粒从而起到加强粘结的作用，有助于提高陶瓷的耐磨能力和抗弯能力。
优选的，所述生物炭为粒径为8-15微米的碳化稻壳粉。
将稻壳加热到着火点温度以下可制得碳化稻壳，其主要成分是碳和二氧化硅，而且活性很高，以碳化稻壳为原料可制备出碳化硅晶须，用于加固和硬化碳化硅陶瓷材料，效果十分显著。
本发明的技术方案之二，上述的碳化物基陶瓷材料的制备方法，包括以下步骤：
(1)将碳化硅粉、硅粉、Ti-Si-Fe合金粉、生物炭、粘结剂混匀后置于球磨机中，加入球磨球进行球磨；
(2)步骤(1)所得球磨料置于喷雾造粒机中，通过控制喷雾造粒工艺参数制得造粒粉料，造粒粉料置于模具中在120-180MPa的压力下压制成型；
(3)步骤(2)成型后的试样在300-500℃条件下固化12-24h后，在氮气气氛，800-1000℃条件下保温1-3h，然后升温至1300-1450℃高温烧结2-5h，冷却至室温得碳化物基陶瓷材料。
优选的，步骤(1)中，所述球磨球为氧化锆球，球料比为3-5∶1，球磨转速为150-200r/min，球磨时间2-4h。
优选的，步骤(1)中，将碳化硅粉、硅粉、Ti-Si-Fe合金粉、生物炭、粘结剂加入溶剂混匀后置于球磨机中，进行球磨，所述溶剂为无水乙醇，加入量为刚好没过原料和球磨球。
在球磨过程中加入少量溶剂可以有效提高各组分在碳化硅中的分散程度，从而提高陶瓷结构的致密性和稳定性，从而提高产品的机械强度。
优选的，步骤(2)中所得造粒粉料平均粒度低于1μm，所述模具为φ(10-50mm)×(30-50mm)圆柱型或(10-25mm)×(10-25mm)×(30-50mm)的长条形。
优选的，步骤(3)中以30-50℃/min的升温速率升温至800-1000℃保温1-3h，然后以50-100℃/min的升温速率升温至1300-1450℃高温烧结2-5h后，以30-50℃/min的降温速率降至室温。
与现有技术相比，本发明具有以下技术效果：
(1)本发明以碳化硅粉、硅粉，Ti-Si-Fe合金粉，生物炭、粘结剂为原料在经过球磨使其充分混合后由喷雾造粒机制备成喷雾粉料，在细化原料的同时获得球形粉体，增强粉体流动性，使其易于后续压制成型；然后将压制成型的原料在氮气氛围下进行高温煅烧，Ti-Si-Fe合金粉中的主要物相TiSi2、TisSi3在氮气氛围下和硅粉发生氮化反应，形成TiN、Si3N4，其具有较高的体积膨胀，从而促进试样的致密化。此外，Ti-Si-Fe合金粉中微量的Fe、Mn、V等的存在，会促进Si粉的氮化，也可对晶体的定向生长起到催化作用，促进针状或柱状SiC、Si3N4晶体的形成，晶须的形成也可以对试样的力学性能起到补强作用。
(2)生成的Si3N4和碳化硅相结合形成一种高硬度的非金属材料，具有良好的耐磨性的同时具有高温强度高、抗高温蠕变能力和抗渣侵蚀能力强、热震稳定性好等优异性能，抗氧化性能也较好。氮化硅结合碳化硅的陶瓷材料的热膨胀系数较低，并具有比碳化硅制品更高的热导率，因此在高温下使用时不容易产生热应力，抗热震性良好。
(3)生物碳的引入，能够在高温下与硅粉表面的氧化膜发生反应，形成SiO、CO，从而破坏硅粉表面的氧化膜，有利于硅粉的氮化。同时添加的生物碳能够与烧成气氛中存在的氧反应形成网络孔洞，成为N2渗透的通道，进而提高了试样的氮化程度，从而显著提高碳化物基陶瓷材料的致密性。
(4)以碳化稻壳为原料在高温煅烧过程中会形成碳化硅晶须，和碳化硅原料形成的SiC颗粒/晶须增韧相快速进入生成的Si3N4晶界中，提高试样在的抗蠕变性能。
(5)本发明制备的碳化物基陶瓷材料在高温条件下具有极好的硬度、密度及强度，克服了现有技术中碳化物基陶瓷材料烧结过程中，碳化硅扩散困难，导致碳化硅的成型速度以及致密性降低，从而影响碳化硅的烧结性能，导致各方面性能无法满足工业化生产的需求的技术问题。
具体实施方式
现详细说明本发明的多种示例性实施方式，该详细说明不应认为是对本发明的限制，而应理解为是对本发明的某些方面、特性和实施方案的更详细的描述。
应理解本发明中所述的术语仅仅是为描述特别的实施方式，并非用于限制本发明。另外，对于本发明中的数值范围，应理解为还具体公开了该范围的上限和下限之间的每个中间值。在任何陈述值或陈述范围内的中间值以及任何其他陈述值或在所述范围内的中间值之间的每个较小的范围也包括在本发明内。这些较小范围的上限和下限可独立地包括或排除在范围内。
除非另有说明，否则本文使用的所有技术和科学术语具有本发明所述领域的常规技术人员通常理解的相同含义。虽然本发明仅描述了优选的方法和材料，但是在本发明的实施或测试中也可以使用与本文所述相似或等同的任何方法和材料。本说明书中提到的所有文献通过引用并入，用以公开和描述与所述文献相关的方法和/或材料。在与任何并入的文献冲突时，以本说明书的内容为准。
在不背离本发明的范围或精神的情况下，可对本发明说明书的具体实施方式做多种改进和变化，这对本领域技术人员而言是显而易见的。由本发明的说明书得到的其他实施方式对技术人员而言是显而易见得的。本申请说明书和实施例仅是示例性的。
关于本文中所使用的“包含”、“包括”、“具有”、“含有”等等，均为开放性的用语，即意指包含但不限于。
本发明中所述的“份”如无特别说明，均按质量份计。
以下实施例中所用粘结剂为1-3μm的氧化铝和二氧化硅按照1∶3的质量比混合而成。
实施例1
(1)取粒径为15-20μm的碳化硅粉50份，0.5-2μm硅粉12份，0.2-0.8μm的Ti-Si-Fe合金粉3份，生物炭15份，粘结剂8份加入适量的无水乙醇后置于球磨机中，按照球料比为4∶1加入氧化锆球，在180r/min的转速下球磨2h；
(2)球磨料置于喷雾造粒机中，制得平均粒度低于1μm的造粒粉料，造粒粉料置于50mm×50mm的圆柱型模具中在150MPa的压力下压制成型；
(3)将压制成型的棒料在500℃条件下固化24h后，通入氮气气氛，50℃/min升温速率升温至1000℃，保温3h，然后100℃/min的升温速率升温至1300℃高温烧结5h，50℃/min的降温速率降至室温，得碳化物基陶瓷材料。
实施例2
(1)取粒径为15-20μm的碳化硅粉60份，0.5-2μm硅粉15份，0.2-0.8μm的Ti-Si-Fe合金粉3份，生物炭20份，粘结剂9份加入适量的无水乙醇后置于球磨机中，按照球料比为5∶1加入氧化锆球，在200r/min的转速下球磨4h；
(2)球磨料置于喷雾造粒机中，制得平均粒度低于1μm的造粒粉料，造粒粉料置于25mm×25mm×50mm的长条型模具中在180MPa的压力下压制成型；
(3)将压制成型的棒料在300℃条件下固化24h后，通入氮气气氛，30℃/min升温速率升温至900℃，保温2h，然后80℃/min的升温速率升温至1400℃高温烧结4h，30℃/min的降温速率降至室温，得碳化物基陶瓷材料。
实施例3
(1)取粒径为15-20μm的碳化硅粉80份，0.5-2μm硅粉18份，0.2-0.8μm的Ti-Si-Fe合金粉3份，生物炭15份，粘结剂8份加入适量的无水乙醇后置于球磨机中，按照球料比为4∶1加入氧化锆球，在150r/min的转速下球磨3h；
(2)球磨料置于喷雾造粒机中，制得平均粒度低于1μm的造粒粉料，造粒粉料置于15mm×15mm×50mm的长条型模具中在150MPa的压力下压制成型；
(3)将压制成型的棒料在400℃条件下固化24h后，通入氮气气氛，50℃/min升温速率升温至950℃，保温3h，然后100℃/min的升温速率升温至1450℃高温烧结3h，50℃/min的降温速率降至室温，得碳化物基陶瓷材料。
对比例1
同实施例1，区别在于，未加入Ti-Si-Fe合金粉。
对比例2
同实施例1，区别在于，未加入生物炭。
对比例3
同实施例1，区别在于，未加入硅粉。
对比例4
同实施例1，区别在于，步骤(3)中未进行固化。
对比例5
同实施例1，区别在于，步骤(3)中煅烧过程未在氮气气氛中进行。
对比例6
同实施例1，区别在于，未进行步骤(2)喷雾造粒粉料。
对比例7
同实施例1，区别在于，步骤(3)中直接100℃/min的升温速率升温至1450℃高温烧结5h。
对实施例1-3，对比例1-7所制备的碳化物基陶瓷材料进行性能测试，结果如表1所示，密度按照GB/T 2413-1981测试，室温弯曲强度按照GB/T 6569-2006测试，硬度按照维氏硬度压痕法测试。
表1
Figure BDA0002473423820000061
由表1可得，本发明提供的碳化物基陶瓷材料具有极好的硬度、密度及强度，且各个参数及配比密切相关，本发明所取得的技术效果是本发明原料、配比及其制备方法的配合得到的。
以上所述的实施例仅是对本发明的优选方式进行描述，并非对本发明的范围进行限定，在不脱离本发明设计精神的前提下，本领域普通技术人员对本发明的技术方案做出的各种变形和改进，均应落入本发明权利要求书确定的保护范围内。

Claims (9)

1.一种碳化物基陶瓷材料，其特征在于，以质量份数计，原料包括以下组分：碳化硅粉50-80份、硅粉10-18份、Ti-Si-Fe合金粉3-5份、生物炭15-20份、粘结剂8-10份。
2.根据权利要求1所述的一种碳化物基陶瓷材料，其特征在于，所述碳化硅粉粒径为15-20μm，硅粉粒径0.5-2μm，Ti-Si-Fe合金粉粒径0.2-0.8μm。
3.根据权利要求1所述的一种碳化物基陶瓷材料，其特征在于，所述粘结剂为氧化铝和二氧化硅按照1∶(3-5)的质量比混合而成，氧化铝、二氧化硅粒径1-3μm。
4.根据权利要求1所述的一种碳化物基陶瓷材料，其特征在于，所述生物炭为粒径为8-15微米的碳化稻壳粉。
5.一种根据权利要求1-4任一项所述的碳化物基陶瓷材料的制备方法，其特征在于，包括以下步骤：
(1)将碳化硅粉、硅粉、Ti-Si-Fe合金粉、生物炭、粘结剂混匀后置于球磨机中，加入球磨球进行球磨；
(2)步骤(1)所得球磨料置于喷雾造粒机中，制得造粒粉料，造粒粉料置于模具中在120-180MPa的压力下压制成型；
(3)步骤(2)成型后的试样在300-500℃条件下固化12-24h后，在氮气气氛，800-1000℃条件下保温1-3h，然后升温至1300-1450℃高温烧结2-5h，冷却至室温得碳化物基陶瓷材料。
6.根据权利要求5所述的碳化物基陶瓷材料的制备方法，其特征在于，步骤(1)中，所述球磨球为氧化锆球，球料比为3-5∶1，球磨转速为150-200r/min，球磨时间2-4h。
7.根据权利要求5所述的碳化物基陶瓷材料的制备方法，其特征在于，步骤(1)中，将碳化硅粉、硅粉、Ti-Si-Fe合金粉、生物炭、粘结剂加入溶剂混匀后置于球磨机中，进行球磨，所述溶剂为无水乙醇，加入量为刚好没过原料和球磨球。
8.根据权利要求5所述的碳化物基陶瓷材料的制备方法，其特征在于，步骤(2)中所得造粒粉料平均粒度低于1μm，所述模具为φ(10-50mm)×(30-50mm)圆柱型或(10-25mm)×(10-25mm)×(30-50mm)的长条形。
9.根据权利要求5所述的碳化物基陶瓷材料的制备方法，其特征在于，步骤(3)中以30-50℃/min的升温速率升温至800-1000℃保温1-3h，然后以50-100℃/min的升温速率升温至1300-1450℃高温烧结2-5h后，以30-50℃/min的降温速率降至室温。
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