CN112500167A - 一种致密化碳化钛复合陶瓷的制备方法 - Google Patents

一种致密化碳化钛复合陶瓷的制备方法 Download PDF

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CN112500167A
CN112500167A CN202011607845.9A CN202011607845A CN112500167A CN 112500167 A CN112500167 A CN 112500167A CN 202011607845 A CN202011607845 A CN 202011607845A CN 112500167 A CN112500167 A CN 112500167A
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titanium carbide
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茹红强
孙卫康
王春华
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Shandong Dongda New Materials Research Institute Co ltd
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Abstract

本发明提供一种致密化碳化钛复合陶瓷的制备方法,所述复合陶瓷的原料中,TiC粉、添加剂、烧结助剂、钛源、C源的质量比为(30‑80):(0‑75):(0‑30):(0‑35):(0‑25),在原料中,引入钛源、C源,通过原位反应,在碳化钛陶瓷基体中合成超细的碳化钛晶粒,提高了硼化锆的烧结活性,有利于致密化,相对密度95%以上;同时引入添加剂和烧结助剂,有利于形成液相,促进碳化钛颗粒之间重新排列,便于形成烧结颈,本发明制得的TiC复合陶瓷材料具有致密度高、高硬度、高韧性、低电阻率等性能,便于大规模自动化生产。

Description

一种致密化碳化钛复合陶瓷的制备方法
技术领域
本发明属于陶瓷材料技术领域,具体涉及一种致密化碳化钛复合陶瓷的制备方法。
背景技术
碳化钛陶瓷具有强度高、导热良好、低电阻率、抗高温氧化、耐化学腐蚀等优良的特性,经常被用在切削刀具、耐磨部件、电接触部件、核聚变反应堆等领域。但是碳化钛属于超硬材料,难以烧结致密化。
目前,虽然使用热压、SPS、自蔓延等烧结方式可以获得致密化的碳化钛复合陶瓷;但是,采用热压烧结工艺,产品上下两面要承受很大的压力,产品的形状往往是板材或片材,形状简单不能复杂,所以形状受到限制;此外,由于产品受压的原因,每一批次烧结的产品数量也会受到限制。SPS和自蔓延烧结工艺,虽然对产品的形状没有要求,但是这两种烧结工艺限定了烧结炉内腔尺寸非常小,产量极其低下,目前只限于实验科研研究,也不适用于大批量工业化生产。
发明专利 CN102390999A公开一种液相烧结SiC-TiC复合陶瓷及其制备方法,由15~50wt%的碳化钛,40~80wt%的碳化硅,5~10wt%的助烧结剂Al2O3和Y2O3组成,经配料、制浆、成型、干燥、烧结而得到,SiC-TiC复合陶瓷的常温抗折强度提高到580Mpa,断裂韧性提高到7.8MPa·m1/2,但是,该方法制备的陶瓷致密度并不高。
发明专利 CN110330318A公开一种微纳复合陶瓷材料,以微米氧化铝为基体,以微米碳化钨和纳米碳化钛为第二相材料,以石墨烯为强韧化相,该种氧化铝-碳化钨-碳化钛-石墨烯微纳复合陶瓷材料,抗弯强度550.92±25.55MPa,硬度23.54±0.63GPa,断裂韧性8.76±0.51MPa·m 1/2,但是,其采用热压烧结工艺,样品虽然能获得较高的综合性能,但是样品的形状、尺寸和数量受到了极大的限制,不适用于规模化大批量生产。
发明内容
为解决现有技术存在的问题,对现有工艺进行进一步优化,本发明提供一种致密化碳化钛复合陶瓷的制备方法,以实现制备具有高致密度、形状可塑性强、便于大规模量产的碳化钛复合陶瓷的发明目的。
为解决以上技术问题,本发明采用以下技术方案:
一种致密化碳化钛复合陶瓷的制备方法,其特征在于,所述复合陶瓷的原料,包括TiC粉、添加剂、烧结助剂、钛源、C源,所述TiC粉、添加剂、烧结助剂、钛源、C源的质量比为(30-80):(0-75):(0-30):(0-35):(0-25);
所述添加剂可以是碳化钨、碳化硅、碳化硼、氧化铝、氧化硅、氮化硅、氮化铝中的一种或几种;
所述TiC粉平均粒度为0.4~5μm,纯度大于96%;
所述C源可以是酚醛树脂、石墨粉、炭黑、石墨烯中的一种或几种;
所述钛源可以是Ti粉、TiCl4、TiO2粉、钛酸丁酯中的一种或几种;
所述烧结助剂可以是氧化钙、氧化镁、氧化钇、氧化铈、氧化镧中的一种或几种;
所述制备方法,包括以下步骤:
(1)将原料、结合剂与液体介质一起混合成浆料,在球磨罐中球磨;
(2)将混合浆料进行喷雾造粒或在40~100℃干燥箱中烘干后手工过筛造粒;
(3)将造粒粉放入模具中,经过模压成型制成陶瓷生坯;
(4)将压制好的陶瓷生坯放入100~250℃干燥箱中干燥;
(5)将生坯放入高温烧结中,1800~2150℃下反应烧结获得致密化TiC复合陶瓷材料;
所述原料、结合剂和液体介质的质量比为100:(20-150):(120-180);
所述结合剂可以是酚醛树脂、PVA或PVB;
所述液体介质可以是水、丙酮或乙醇;
所述烧结,烧结气氛可以是真空、氩气、氢气中的一种或两种;
所述过筛造粒,筛网规格为40~100目;
所述模压成型,压力为100~250MPa。
本专利采用无压烧结工艺,样品不用加压,则样品的形状、尺寸和数量不受限制;且在原料中引入钛源和碳源,Ti+C=TiC,TiO2+3C=TiC+2CO,不仅提高的碳化钛的烧结活性,促进致密化,而且超细的碳化钛颗粒对陶瓷基体和形成的液相均有弥散强化作用,从而提高综合性能,使无压烧结工艺得到的综合性能与热压烧结的相近,适用于规模化大批量生产。
采用上述技术方案,本发明的有益效果为:
1、采用本发明致密化碳化钛复合陶瓷的制备方法,在原料中,引入钛源、C源,通过原位反应,在碳化钛陶瓷基体中合成超细的碳化钛晶粒,提高了硼化锆的烧结活性,有利于致密化,相对密度95-99%;
2、采用本发明致密化碳化钛复合陶瓷的制备方法,在原料中,引入添加剂和烧结助剂,有利于形成液相,促进碳化钛颗粒之间重新排列,便于形成烧结颈,从而降低了烧结温度,烧结温度在1850-2150℃;
3、采用本发明致密化碳化钛复合陶瓷的制备方法,提高了复合陶瓷的弯曲强度和断裂韧性,弯曲强度达到485-619MPa,断裂韧性达到4.73-8.12MPa·m1/2;
4、采用本发明致密化碳化钛复合陶瓷的制备方法,降低了碳化钛复合陶瓷的气孔率,气孔率为0.31-0.82%;同时维氏硬度达到19.50-26.09GPa;
5、采用本发明致密化碳化钛复合陶瓷的制备方法,碳化钛复合陶瓷材料的电阻率可达到4.07×10-6-6.44×10-5Ω·m;
6、本发明采用无压烧结工艺,可以制备出形状可塑的产品,工艺简单,对设备要求度低,便于大规模自动化生产,产品成本低且性能高,具有巨大的市场实用价值。
附图说明
图1为本发明实施例1中TiC-SiC复合陶瓷材料条状样品实物图。
图2为本发明实施例1中TiC-SiC复合陶瓷材料金相显微图。
图3为本发明实施例2中TiC-WC复合陶瓷材料条状样品实物图。
图4为本发明实施例2中TiC-WC复合陶瓷材料金相显微图。
图5为本发明实施例2中TiC-WC复合陶瓷材料SEM和EDS图。
图6为本发明实施例3中TiC-Al2O3复合陶瓷材料条状样品实物图。
图7为本发明实施例3中TiC-Al2O3复合陶瓷材料金相显微图。
具体实施方式:
下面结合具体的实施例,进一步阐述本发明。
实施例1
一种致密化碳化钛复合陶瓷的制备方法,步骤如下:
(1)将TiC粉、添加剂碳化硅和氧化铝、烧结助剂氧化钇、Ti粉、石墨烯按质量比50:65:4:10:3混合成混合粉料,将混合粉料、浓度为5%PVA溶液的结合剂、液体介质去离子水按质量比100:20:150一起混合成浆料,在球磨罐中球磨;
所述TiC粉,平均粒度为0.8μm,纯度99.9%;
所述碳化硅与氧化铝质量比为15:1;
(2)将混合浆料进行喷雾造粒;
(3)将造粒粉放入模具中,经压力机模压成型,压力150MPa,获得生坯;
(4)将压制好的陶瓷生坯放入150℃干燥箱中干燥排出体内水分;
(5)将生坯放入烧结中,在真空状态下,升温至1600℃保温30min,之后充氩气,达到烧结温度2150℃时,保温180min,获得TiC-SiC复合陶瓷材料;
本实施例制得的TiC-SiC复合陶瓷材料条状样品如图1所示,金相显微图如图2所示;经测试,该TiC-SiC复合陶瓷材料的相对密度为98.52%、气孔率为0.31%、弯曲强度为619MPa、断裂韧性为8.12MPa·m1/2、维氏硬度为26.09GPa、电阻率为6.44×10-5Ω·m。
实施例2
一种致密化碳化钛复合陶瓷的制备方法,步骤如下:
(1)按质量比,将TiC粉、添加剂碳化钨、烧结助剂氧化铈、氧化钛粉、石墨粉=65:10:5:35:12混合成混合粉料,将混合粉料、浓度为5%酚醛树脂溶液的结合剂、液体介质乙醇=100:30:180一起混合成浆料,在球磨罐中球磨;
所述TiC粉,平均粒度为0.5μm,纯度98.5%;
(2)将球磨后的浆料在80℃干燥箱中烘干后,手工研磨破碎粉末,并过100目筛造粒;
(3)将造粒粉放入模具中,经压力机模压成型,压力200MPa,获得生坯;
(4)将压制好的陶瓷生坯放入200℃干燥箱中干燥排出体内水分;
(5)将生坯放入烧结中,在真空状态下,升温至1550℃保温60min,达到烧结温度2050℃时,保温120min,获得TiC-WC复合陶瓷材料;
本实施例制得的TiC-WC复合陶瓷材料条状样品如图3所示,金相显微图如图4所示,SEM与EDS如图5所示;经测试,该TiC-WC复合陶瓷材料的相对密度为95.73%、气孔率为0.82%、弯曲强度为525MPa、断裂韧性为7.17MPa·m1/2、维氏硬度为25.78GPa、电阻率为4.07×10-6Ω·m。
实施例3
一种致密化碳化钛复合陶瓷的制备方法,步骤如下:
(1)按质量比,将TiC粉、添加剂氧化铝、烧结助剂氧化镁、氧化钛粉、炭黑=55:35:5:18:9混合成混合粉料,将混合粉料、浓度为5%PVB的结合剂、液体介质丙酮=100:150:120一起混合成浆料,在球磨罐中球磨;
所述TiC粉,平均粒度为1.0μm,纯度99%;
(2)将球磨后的浆料在100℃干燥箱中烘干后,手工研磨破碎粉末,并过80目筛造粒;
(3)将造粒粉放入模具中,经压力机模压成型,压力250MPa,获得生坯;
(4)将压制好的陶瓷生坯放入250℃干燥箱中干燥排出体内水分;
(5)将生坯放入烧结中,在氩气状态下,升温至1300℃保温60min,达到烧结温度1850℃时,保温90min,获得TiC-Al2O3复合陶瓷材料;
本实施例制得的TiC-Al2O3复合陶瓷材料条状样品如图6所示,金相显微图如图7所示;经测试,该TiC-Al2O3复合陶瓷材料的相对密度为97.14%、气孔率为0.72%、弯曲强度为485MPa、断裂韧性为4.37MPa·m1/2、维氏硬度为19.50GPa、电阻率为7.62×10-6Ω·m。
以上所述,仅为本发明的实施例,并非用以限定本发明的范围,本发明的上述实施例还可以做出各种变化。凡是依据本发明申请的权利要求书及说明书内容所作的简单、等效变化与修饰,皆落入本发明专利的权利要求保护范围。本发明未详尽描述的均为常规技术内容。

Claims (11)

1.一种致密化碳化钛复合陶瓷的制备方法,其特征在于,所述复合陶瓷的原料,包括TiC粉、添加剂、烧结助剂、钛源、C源,所述TiC粉、添加剂、烧结助剂、钛源、C源的质量比为(30-80):(0-75):(0-30):(0-35):(0-25)。
2.根据权利要求1所述的制备方法,其特征在于,所述添加剂可以是碳化钨、碳化硅、碳化硼、氧化铝、氧化硅、氮化硅、氮化铝中的一种或几种。
3.根据权利要求1所述的制备方法,其特征在于,所述TiC粉平均粒度为0.4-5μm,纯度大于96%。
4.根据权利要求1所述的制备方法,其特征在于,所述C源可以是酚醛树脂、石墨粉、炭黑、石墨烯中的一种或几种。
5.根据权利要求1所述的制备方法,其特征在于,所述钛源可以是Ti粉、TiCl4、TiO2粉、钛酸丁酯中的一种或几种。
6.根据权利要求1所述的制备方法,其特征在于,所述烧结助剂可以是氧化钙、氧化镁、氧化钇、氧化铈、氧化镧中的一种或几种。
7.根据权利要求1所述的制备方法,其特征在于,所述制备方法,包括将原料与结合剂和液体介质混合成浆料,所述原料、结合剂和液体介质的质量比为100:(20-150):(120-180)。
8.根据权利要求7所述的制备方法,其特征在于,所述结合剂可以是酚醛树脂、PVA或PVB;所述液体介质可以是水、丙酮或乙醇。
9.根据权利要求7所述的制备方法,其特征在于,所述制备方法,包括烧结,所述烧结,烧结气氛可以是真空、氩气、氢气中的一种或两种。
10.根据权利要求7所述的制备方法,其特征在于,所述制备方法,包括过筛造粒,所述过筛造粒,筛网规格为40-100目。
11.根据权利要求7所述的制备方法,其特征在于,所述制备方法,包括模压成型,所述模压成型,压力为100-250MPa。
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114292107A (zh) * 2022-01-20 2022-04-08 山东东大新材料研究院有限公司 一种用于电火花线切割设备的陶瓷导电块及其制备方法
CN115196966A (zh) * 2021-04-12 2022-10-18 中国科学院上海硅酸盐研究所 一种温阻特性恒定的碳化硅复相陶瓷及其制备方法
CN115287516A (zh) * 2022-07-22 2022-11-04 燕山大学 高熵陶瓷结合的wc硬质合金及其制备方法

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006106873A1 (ja) * 2005-03-30 2006-10-12 Fukuoka Prefecture 炭化チタン粉末および炭化チタン-セラミックス複合粉末とその製造方法ならびにその炭化チタン粉末の焼結体および炭化チタン-セラミックス複合粉末の焼結体とその製造方法
CN101723671A (zh) * 2009-12-03 2010-06-09 陕西科技大学 一种TiC/Al2O3复合材料及其制备方法
CN102249697A (zh) * 2010-05-17 2011-11-23 中国科学院上海硅酸盐研究所 反应助剂促进烧结硼化钛陶瓷的方法
CN102390999A (zh) * 2011-08-10 2012-03-28 武汉钢铁(集团)公司 液相烧结SiC-TiC复合陶瓷及其制备方法
CN105174962A (zh) * 2015-09-11 2015-12-23 杨洋 一种高强度高温钛陶瓷及其制备方法
CN105481365A (zh) * 2014-09-15 2016-04-13 中国科学院上海硅酸盐研究所 一种高致密化碳化钛陶瓷的制备方法
CN108440014A (zh) * 2018-04-24 2018-08-24 莱芜职业技术学院 一种采用反应烧结法制备多孔碳化钛陶瓷的方法
CN111848163A (zh) * 2020-07-30 2020-10-30 山东东大新材料研究院有限公司 一种电阻率、气孔率、颜色可调氧化锆陶瓷及其制备方法

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006106873A1 (ja) * 2005-03-30 2006-10-12 Fukuoka Prefecture 炭化チタン粉末および炭化チタン-セラミックス複合粉末とその製造方法ならびにその炭化チタン粉末の焼結体および炭化チタン-セラミックス複合粉末の焼結体とその製造方法
CN101723671A (zh) * 2009-12-03 2010-06-09 陕西科技大学 一种TiC/Al2O3复合材料及其制备方法
CN102249697A (zh) * 2010-05-17 2011-11-23 中国科学院上海硅酸盐研究所 反应助剂促进烧结硼化钛陶瓷的方法
CN102390999A (zh) * 2011-08-10 2012-03-28 武汉钢铁(集团)公司 液相烧结SiC-TiC复合陶瓷及其制备方法
CN105481365A (zh) * 2014-09-15 2016-04-13 中国科学院上海硅酸盐研究所 一种高致密化碳化钛陶瓷的制备方法
CN105174962A (zh) * 2015-09-11 2015-12-23 杨洋 一种高强度高温钛陶瓷及其制备方法
CN108440014A (zh) * 2018-04-24 2018-08-24 莱芜职业技术学院 一种采用反应烧结法制备多孔碳化钛陶瓷的方法
CN111848163A (zh) * 2020-07-30 2020-10-30 山东东大新材料研究院有限公司 一种电阻率、气孔率、颜色可调氧化锆陶瓷及其制备方法

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
曲远方等: "《现代陶瓷材料及技术》", 31 May 2008, 华东理工大学出版社, pages: 487 *
薛云飞等, 北京理工大学出版社, pages: 195 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115196966A (zh) * 2021-04-12 2022-10-18 中国科学院上海硅酸盐研究所 一种温阻特性恒定的碳化硅复相陶瓷及其制备方法
CN115196966B (zh) * 2021-04-12 2023-05-09 中国科学院上海硅酸盐研究所 一种温阻特性恒定的碳化硅复相陶瓷及其制备方法
CN114292107A (zh) * 2022-01-20 2022-04-08 山东东大新材料研究院有限公司 一种用于电火花线切割设备的陶瓷导电块及其制备方法
CN115287516A (zh) * 2022-07-22 2022-11-04 燕山大学 高熵陶瓷结合的wc硬质合金及其制备方法

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