CN111848170A - 一种碳化硼基复合陶瓷材料及其制备方法 - Google Patents
一种碳化硼基复合陶瓷材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种碳化硼基复合陶瓷材料及其制备方法,该复合陶瓷材料由B4C粉末、Ti3SiC2粉末及金属氢化物粉末经压力烧结制备而成。本发明在较低的烧结温度和较短的烧结保温时间下,获得了高致密度、高硬度、高弯曲强度和断裂韧性、可电火花线切割加工的碳化硼基复合陶瓷材料,改善了碳化硼陶瓷的力学性能和加工性能,具有较高的实用价值。
Description
技术领域
本发明涉及一种碳化硼(B4C)基复合陶瓷材料及其制备工艺,属于陶瓷基复合材料反应烧结制备领域。
背景技术
碳化硼(B4C)陶瓷因具有一系列优异的化学和物理性能,如良好的化学稳定性、高硬度、低密度、高熔点和良好的耐磨性,在防弹装甲、耐火材料、磨料涂层、电子等领域有广阔的应用前景,同时由于硼元素具有良好的中子吸收能力,B4C陶瓷可用于核反应堆中作为中子吸收剂和屏蔽材料使用。然而,由于B4C陶瓷的烧结性极差,一般需要烧结温度到达2200℃且保温时间不低于30min,这导致了B4C陶瓷晶粒组织易变得粗大,降低了陶瓷材料的综合力学性能。此外,B4C陶瓷的机械加工性能差、脆性大、断裂韧性差等问题,也限制了B4C陶瓷的应用。因此,研究和发展B4C基复合陶瓷材料,探索B4C基复合陶瓷材料的烧结制备工艺具有重要的意义。
B4C陶瓷的烧结性能差归因于其B-C之间的高共价键和原子之间低扩散迁移率,机械加工性能差归因于其高硬度和低电导率,脆性大归因于其对裂纹扩展的高度敏感,所以研究降低B4C陶瓷的烧结温度,提高其断裂韧性及改善其机械加工性能对其应用而言至关重要。 Ti3SiC2是一种具有三元层状的MAX相陶瓷,它综合了金属和陶瓷的诸多优良性能,具有很好的导热性和导电性,相对较低的维氏硬度和较高的弹性模量,且有延展性,同时具有高的屈服强度、高熔点、高热稳定性和良好的抗氧化性能等性能。B4C与Ti3SiC2及金属氢化物在一定条件下能够反应生成SiC、TiB2和金属碳化物。碳化硅(SiC)具有化学性能稳定、硬度高、熔点高、耐磨性能好等特点,能够大幅提高复合陶瓷的抗氧化能力和断裂韧性;二硼化钛(TiB2)具有硬度高、熔点高、热稳定性与抗氧化性能好、耐酸碱腐蚀等特点,且具有良好的导电性,能够提高复合陶瓷的断裂韧性和改善陶瓷的机械加工性能;TiC、ZrC、VC和HfC等金属碳化物具有高熔点、高硬度、良好的导热和导电性能,能够大幅度提高复合陶瓷的机械加工性能。SiC、TiB2和金属碳化物在促进B4C陶瓷烧结致密化的同时,也通过弥散强化等多种机制作用抑制了B4C陶瓷晶粒的长大,对提高复合陶瓷的综合力学性能具有非常显著的作用。因此,使用Ti3SiC2和金属氢化物粉末烧结助剂,利用原位反应生成SiC、TiB2和金属碳化物强韧化相,不仅能够在较低的温度下制备出高致密度的陶瓷材料,且在基体中均匀分布的强韧化相能够有效地抑制B4C晶粒长大,得到综合力学性能优异的复合陶瓷材料。此外,生成的TiB2和金属碳化物强韧化相因具有较高的电导率,使得陶瓷能够用电火花线切割进行加工。研究在较低的烧结温度下,控制添加烧结助剂的含量,制备出具有高致密度、高电导率、综合力学性能优异的B4C基复合陶瓷材料,具有重要的现实意义。
发明内容
为了避免现有技术中存在的不足之处,本发明旨在提供一种高致密度、高电导率、综合力学性能优异的B4C基复合陶瓷材料及其制备方法。
本发明为实现发明目的,采用如下技术方案:
本发明公开了一种碳化硼基复合陶瓷材料,其特点在于:所述复合陶瓷材料是由B4C粉末、Ti3SiC2粉末及金属氢化物粉末经压力烧结制备而成。所述的金属氢化物为TiH2、VH2、 ZrH2和HfH2中的至少一种。
进一步地,所述复合陶瓷材料的原料按质量百分数的配比为:Ti3SiC2粉末10-30wt.%,金属氢化物粉末5-30wt.%,余量为B4C粉末。
本发明所述碳化硼基复合陶瓷材料的制备方法,包括如下步骤:
步骤1、混合粉末的制备
按配比量称取B4C粉末、Ti3SiC2粉末以及金属氢化物粉末,倒入球磨罐中,以无水乙醇为球磨介质,将球磨罐置于行星球磨机中,球磨机的转速为360rpm,球磨混合12h,再置于 50℃真空干燥箱中干燥12h,即得所需混合粉末;
步骤2、压力烧结
准备一个石墨模具或钼包套,将步骤1制取的混合粉末装入石墨模具或钼包套中,再将装配完成的石墨模具或钼包套放入压力烧结炉中进行压力烧结,即得B4C基复合陶瓷材料。
进一步地:步骤1中,所述B4C粉末的粒度为0.5-5μm,纯度不低于96%;所述Ti3SiC2粉末的粒度为0.5-10μm,纯度不低于98%:所述金属氢化物粉末的粒度为0.5-10μm,纯度不低于98%。
进一步地,步骤2中,压力烧结可以为放电等离子烧结、热压烧结或热等静压烧结等常规压力烧结方法。
当采用放电等离子烧结时,烧结粉末用模具为石墨模具,烧结条件为:烧结炉真空状态下,对样品施加压力10MPa并加热升温至700℃保温10min,随后施加压力至30MPa,继续升温至烧结温度并保温,升温速率为50-100℃/min,烧结温度为1700-1800℃,保温时间为10-20min;保温结束后随即降压、降温,样品随炉冷却;
当采用热压烧结时,烧结粉末用模具为石墨模具,烧结条件为:烧结炉真空状态下,以 5-20℃/min的升温速率将样品加热至1700-1850℃,保温时间为60-180min,加载压力为 15-40MPa;保温结束后随即降压、降温,样品随炉冷却;
当采用热等静压烧结时,将混合粉末装入铺有石墨纸的钼包套内,烧结条件为:在氩气下以30-100℃/min的升温速率将样品加热至1600-1800℃,保温时间为60-240min,加载压力为150-300MPa;保温结束后随即降压、降温,样品随炉冷却。
本发明利用原位反应压力烧结方法制备了B4C基复合陶瓷。采用常规的烧结技术,在低温下实现烧结致密,改善碳化硼的烧结性能,提高材料的力学性能,丰富高熵陶瓷体系。制备的复合陶瓷材料中含有TiB2和金属碳化物导电相,可采用电火花线切割进行加工,改善碳化硼陶瓷的机械加工性能。
与现有技术相比,本发明的有益效果体现在:
1、本发明探索了B4C、Ti3SiC2和金属氢化物粉末配比以及压力烧结方法,在较低的烧结温度(1600-1850℃)及较短的烧结保温时间(最短10min)下,制备了高致密度B4C基复合陶瓷。Ti3SiC2和金属氢化物烧结助剂的加入,有效降低了B4C陶瓷的烧结温度、缩短了烧结保温时间,解决了B4C陶瓷烧结温度高及保温时间长等难烧结的问题。
2、本发明在保持B4C陶瓷高强度和高硬度的前提下,通过原位反应生成了晶粒细小且在B4C基体中均匀分布的TiB2、SiC和金属碳化物等强韧化相,促进烧结致密化的同时有效抑制了晶粒长大,解决了B4C陶瓷烧结致密度不高及断裂韧性低的问题。
3、本发明中,由于原位反应生成了较高含量的具有良好电导率的TiB2相和MC(M=Ti, Zr,V,Hf)金属碳化物相,因而B4C-TiB2-SiC-MC多相复合陶瓷可用电火花线切割加工,解决了B4C陶瓷机械加工困难的问题。
附图说明
图1是添加不同质量百分数Ti3SiC2和TiH2粉末制备的B4C基复合陶瓷的XRD图谱。其中,曲线(a)对应实施例1所制备的B4C基复合陶瓷(B4C+11.67wt.%Ti3SiC2+7.5wt.%TiH2);曲线(b)对应实施例2所制备的B4C基复合陶瓷(B4C+15.03wt.%Ti3SiC2+9.6wt.%TiH2);曲线(c)对应实施例3所制备的B4C基复合陶瓷(B4C+18.1wt.%Ti3SiC2+11.56wt.%TiH2);曲线(d)对应实施例4所制备的B4C基复合陶瓷(B4C+21.1wt.%Ti3SiC2+13.39wt.%TiH2)。从图1可以看出添加不同含量Ti3SiC2和TiH2粉末所制备出的复合陶瓷材料,在烧结温度 1750℃、压力30MPa、保温时间10min的工艺参数下,都生成了TiB2、SiC和TiC强韧化相。
具体实施方式
以下结合具体的实施例对本发明的技术方案作进一步的分析说明。
下述实施例中,所用B4C粉末的粒度为0.5-5μm、纯度≥97%,所用Ti3SiC2粉末的粒度为 0.5-10μm,纯度≥98%,所用TiH2粉末的粒度为0.5-10μm、纯度≥99%,所用ZrH2粉末的粒度为0.5-10μm、纯度≥99%,所用VH2粉末的粒度为0.5-10μm、纯度≥99%,所用HfH2粉末的粒度为0.5-10μm、纯度≥99%。
对比例1
本对比例通过放电等离子烧结技术制备纯B4C陶瓷的工艺如下:
准备一个内径20mm的石墨模具,两个配套的石墨压头,两个石墨垫片,石墨纸;将石墨纸裁出两个直径20mm的圆形石墨纸和一个正好覆盖石墨模具内壁的矩形石墨纸;将矩形石墨纸贴在石墨模具内壁,并按照石墨压头/石墨垫片/石墨纸/碳化硼粉末/石墨纸/石墨垫片/ 石墨压头的顺序进行装配;
将装配完成的石墨模具放入放电等离子烧结炉中,室温下对烧结炉抽真空至20Pa以下,对样品加载压力10MPa并加热升温至700℃保温10min,随后施加压力至30MPa,以100℃/min 的升温速率继续升温至1750℃并保温10min,保温结束后随即降压、降温,样品随炉冷却。
经测试,如表1所示,本实施例所得的B4C基复合陶瓷材料的相对密度、维氏硬度、断裂韧性、弯曲强度分别为85.4%、7.9GPa、2.9MPa·m1/2、182.7MPa。
实施例1
本实施例通过原位反应放电等离子烧结技术制备B4C基复合陶瓷材料的工艺如下:
步骤1、混合粉末的制备
按照质量百分数,称取80.83wt.%B4C粉末、11.67wt.%Ti3SiC2粉末和7.5wt.%TiH2粉末,将三种粉末倒入球磨罐中,以无水乙醇为球磨介质,将球磨罐置于行星球磨机中,球磨机的转速为360rpm,球磨12h至完全混合均匀,随后置于真空干燥箱中50℃干燥12h,即得反应烧结混合粉末;
步骤2、放电等离子烧结
准备一个内径20mm的石墨模具,两个配套的石墨压头,两个石墨垫片,石墨纸;将石墨纸裁出两个直径20mm的圆形石墨纸和一个正好覆盖石墨模具内壁的矩形石墨纸;将矩形石墨纸贴在石墨模具内壁,并按照石墨压头/石墨垫片/石墨纸/反应烧结混合粉末/石墨纸/石墨垫片/石墨压头的顺序进行装配;
将装配完成的石墨模具放入放电等离子烧结炉中,室温下对烧结炉抽真空至20Pa以下,对样品加载压力10MPa并加热升温至700℃保温10min,随后施加压力至30MPa,以100℃/min 的升温速率继续升温至1750℃并保温10min,保温结束后随即降压、降温,样品随炉冷却。
经测试,如表1所示,本实施例所得的B4C基复合陶瓷材料的相对密度、维氏硬度、断裂韧性、弯曲强度分别为94.3%、22.3GPa、5.6MPa·m1/2、395.4MPa。
实施例2
本实施例通过原位反应放电等离子烧结技术制备B4C基复合陶瓷材料的工艺如下:
步骤1、混合粉末的制备
按照质量百分数,称取75.37wt.%B4C粉末、15.03wt.%Ti3SiC2粉末和9.6wt.%TiH2,将三种粉末倒入球磨罐中,以无水乙醇为球磨介质,将球磨罐置于行星球磨机中,球磨机的转速为360rpm,球磨12h至完全混合均匀,随后置于真空干燥箱中50℃干燥12h,即得反应烧结混合粉末;
步骤2、放电等离子烧结
准备一个内径20mm的石墨模具,两个配套的石墨压头,两个石墨垫片,石墨纸;将石墨纸裁出两个直径20mm的圆形石墨纸和一个正好覆盖石墨模具内壁的矩形石墨纸;将矩形石墨纸贴在石墨模具内壁,并按照石墨压头/石墨垫片/石墨纸/反应烧结混合粉末/石墨纸/石墨垫片/石墨压头的顺序进行装配;
将装配完成的石墨模具放入放电等离子烧结炉中,室温下对烧结炉抽真空至20Pa以下,对样品加载压力10MPa并加热升温至700℃保温10min,随后施加压力至30MPa,以100℃/min 的升温速率继续升温至1750℃并保温10min,保温结束后随即降压、降温,样品随炉冷却。
经测试,如表1所示,本实施例所得B4C基复合陶瓷材料的相对密度、维氏硬度、断裂韧性、弯曲强度分别为95.8%、25.7GPa、6.9MPa·m1/2、436.8MPa。
实施例3
本实施例通过原位反应放电等离子烧结技术制备B4C基复合陶瓷材料的工艺如下:
步骤1、混合粉末的制备
按照质量百分数,称取70.34wt.%B4C粉末、18.1wt.%Ti3SiC2粉末和11.56wt.%TiH2粉末,将三种粉末倒入球磨罐中,以无水乙醇为球磨介质,将球磨罐置于行星球磨机中,球磨机的转速为360rpm,球磨12h至完全混合均匀,随后置于真空干燥箱中50℃干燥12h,即得反应烧结混合粉末;
步骤2、放电等离子烧结
准备一个内径20mm的石墨模具,两个配套的石墨压头,两个石墨垫片,石墨纸;将石墨纸裁出两个直径20mm的圆形石墨纸和一个正好覆盖石墨模具内壁的矩形石墨纸;将矩形石墨纸贴在石墨模具内壁,并按照石墨压头/石墨垫片/石墨纸/反应烧结混合粉末/石墨纸/石墨垫片/石墨压头的顺序进行装配;
将装配完成的石墨模具放入放电等离子烧结炉中,室温下对烧结炉抽真空至20Pa以下,对样品加载压力10MPa并加热升温至700℃保温10min,随后施加压力至30MPa,以100℃/min 的升温速率继续升温至1750℃并保温10min,保温结束后随即降压、降温,样品随炉冷却。
经测试,如表1所示,本实施例所得B4C基复合陶瓷材料的相对密度、维氏硬度、断裂韧性、弯曲强度分别为96.4%、29.6GPa、8.2MPa·m1/2、492.7MPa。
实施例4
本实施例通过原位反应放电等离子烧结技术制备B4C基复合陶瓷材料的工艺如下:
步骤1、混合粉末的制备
按照质量百分数,称取65.51wt.%B4C粉末、21.1wt.%Ti3SiC2粉末和13.39wt.%TiH2粉末,将三种粉末倒入球磨罐中,以无水乙醇为球磨介质,将球磨罐置于行星球磨机中,球磨机的转速为360rpm,球磨12h至完全混合均匀,随后置于真空干燥箱中50℃干燥12h,即得反应烧结混合粉末;
步骤2、放电等离子烧结
准备一个内径20mm的石墨模具,两个配套的石墨压头,两个石墨垫片,石墨纸;将石墨纸裁出两个直径20mm的圆形石墨纸和一个正好覆盖石墨模具内壁的矩形石墨纸;将矩形石墨纸贴在石墨模具内壁,并按照石墨压头/石墨垫片/石墨纸/反应烧结混合粉末/石墨纸/石墨垫片/石墨压头的顺序进行装配;
将装配完成的石墨模具放入放电等离子烧结炉中,室温下对烧结炉抽真空至20Pa以下,对样品加载压力10MPa并加热升温至700℃保温10min,随后施加压力至30MPa,以100℃/min 的升温速率继续升温至1750℃并保温10min,保温结束后随即降压、降温,样品随炉冷却。
经测试,如表1所示,本实施例所得B4C基复合陶瓷材料的相对密度、维氏硬度、断裂韧性、弯曲强度分别为96.3%、27.4GPa、8.6MPa·m1/2、514.6MPa。
实施例5
本实施例通过原位反应放电等离子烧结技术制备B4C基复合陶瓷材料的工艺如下:
步骤1、混合粉末的制备
按照质量百分数,称取74.6wt.%B4C粉末、15.1wt.%Ti3SiC2粉末和10.3wt.%VH2粉末,将三种粉末倒入球磨罐中,以无水乙醇为球磨介质,将球磨罐置于行星球磨机中,球磨机的转速为360rpm,球磨12h至完全混合均匀,随后置于真空干燥箱中50℃干燥12h,即得反应烧结混合粉末;
步骤2、放电等离子烧结
准备一个内径20mm的石墨模具,两个配套的石墨压头,两个石墨垫片,石墨纸;将石墨纸裁出两个直径20mm的圆形石墨纸和一个正好覆盖石墨模具内壁的矩形石墨纸;将矩形石墨纸贴在石墨模具内壁,并按照石墨压头/石墨垫片/石墨纸/反应烧结混合粉末/石墨纸/石墨垫片/石墨压头的顺序进行装配;
将装配完成的石墨模具放入放电等离子烧结炉中,室温下对烧结炉抽真空至20Pa以下,对样品加载压力10MPa并加热升温至700℃保温10min,随后施加压力至30MPa,以100℃/min 的升温速率继续升温至1750℃并保温10min,保温结束后随即降压、降温,样品随炉冷却。
经测试,如表1所示,本实施例所得B4C基复合陶瓷材料的相对密度、维氏硬度、断裂韧性、弯曲强度分别为97.1%、28.4GPa、7.7MPa·m1/2、484.2MPa。
实施例6
本实施例通过原位反应放电等离子烧结技术制备B4C基复合陶瓷材料的工艺如下:
步骤1、混合粉末的制备
按照质量百分数,称取71.2wt.%B4C粉末、13.2wt.%Ti3SiC2粉末和15.6wt.%ZrH2粉末,将三种粉末倒入球磨罐中,以无水乙醇为球磨介质,将球磨罐置于行星球磨机中,球磨机的转速为360rpm,球磨12h至完全混合均匀,随后置于真空干燥箱中50℃干燥12h,即得反应烧结混合粉末;
步骤2、放电等离子烧结
准备一个内径20mm的石墨模具,两个配套的石墨压头,两个石墨垫片,石墨纸;将石墨纸裁出两个直径20mm的圆形石墨纸和一个正好覆盖石墨模具内壁的矩形石墨纸;将矩形石墨纸贴在石墨模具内壁,并按照石墨压头/石墨垫片/石墨纸/反应烧结混合粉末/石墨纸/石墨垫片/石墨压头的顺序进行装配;
将装配完成的石墨模具放入放电等离子烧结炉中,室温下对烧结炉抽真空至20Pa以下,对样品加载压力10MPa并加热升温至700℃保温10min,随后施加压力至30MPa,以100℃/min 的升温速率继续升温至1750℃并保温10min,保温结束后随即降压、降温,样品随炉冷却。
经测试,如表1所示,本实施例所得B4C基复合陶瓷材料的相对密度、维氏硬度、断裂韧性、弯曲强度分别为96.2%、30.8GPa、7.9MPa·m1/2、491.5MPa。
实施例7
本实施例通过原位反应放电等离子烧结技术制备B4C基复合陶瓷材料的工艺如下:
步骤1、混合粉末的制备
按照质量百分数,称取61.9wt.%B4C粉末、11.5wt.%Ti3SiC2粉末和26.6wt.%HfH2粉末,将三种粉末倒入球磨罐中,以无水乙醇为球磨介质,将球磨罐置于行星球磨机中,球磨机的转速为360rpm,球磨12h至完全混合均匀,随后置于真空干燥箱中50℃干燥12h,即得反应烧结混合粉末;
步骤2、放电等离子烧结
准备一个内径20mm的石墨模具,两个配套的石墨压头,两个石墨垫片,石墨纸;将石墨纸裁出两个直径20mm的圆形石墨纸和一个正好覆盖石墨模具内壁的矩形石墨纸;将矩形石墨纸贴在石墨模具内壁,并按照石墨压头/石墨垫片/石墨纸/反应烧结混合粉末/石墨纸/石墨垫片/石墨压头的顺序进行装配;
将装配完成的石墨模具放入放电等离子烧结炉中,室温下对烧结炉抽真空至20Pa以下,对样品加载压力10MPa并加热升温至700℃保温10min,随后施加压力至30MPa,以100℃/min 的升温速率继续升温至1750℃并保温10min,保温结束后随即降压、降温,样品随炉冷却。
经测试,如表1所示,本实施例所得B4C基复合陶瓷材料的相对密度、维氏硬度、断裂韧性、弯曲强度分别为97.4%、29.4GPa、7.3MPa·m1/2、472.4MPa。
各实施例结果总结:
本发明利用B4C粉末与Ti3SiC2粉末及金属氢化物粉末原位反应,在B4C基体中形成TiB2、 SiC和MC碳化物(M=Ti,V,Zr,Hf)等强韧化相,获得了高致密度、综合力学性能优良、电导率良好的B4C-TiB2-SiC-MC多相复合陶瓷。Ti3SiC2和金属氢化物烧结助剂的加入,在较低的烧结温度和较短的烧结保温时间下,通过原位反应生成了晶粒细小且在B4C基体中分布均匀的TiB2、SiC和MC强韧化相,促进烧结致密化的同时有效抑制了B4C晶粒长大,提高了材料的综合力学性能。此外,B4C-TiB2-SiC-MC多相复合陶瓷具有较高的电导率,可使用电火花线切割进行加工。本发明可以制备综合力学性能优异、高电导率的B4C基复合陶瓷材料,解决了B4C基复合陶瓷制备及应用的一个技术问题。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (7)
1.一种碳化硼基复合陶瓷材料,其特征在于:所述复合陶瓷材料是由B4C粉末、Ti3SiC2粉末及金属氢化物粉末经压力烧结制备而成。
2.根据权利要求1所述的碳化硼基复合陶瓷材料,其特征在于:所述的金属氢化物为TiH2、VH2、ZrH2和HfH2中的至少一种。
3.根据权利要求1或2所述的碳化硼基复合陶瓷材料,其特征在于,所述复合陶瓷材料的原料按质量百分数的配比为:Ti3SiC2粉末10-30wt.%,金属氢化物粉末5-30wt.%,余量为B4C粉末。
4.一种权利要求1~3中任意一项所述碳化硼基复合陶瓷材料的制备方法,其特征在于,包括如下步骤:
步骤1、混合粉末的制备
按配比量称取B4C粉末、Ti3SiC2粉末以及金属氢化物粉末,倒入球磨罐中,以无水乙醇为球磨介质,将球磨罐置于行星球磨机中,球磨机的转速为360rpm,球磨混合12h,再置于50℃真空干燥箱中干燥12h,即得所需混合粉末;
步骤2、压力烧结
将所述混合粉末装配至石墨模具或钼包套中,再将装配完成的石墨模具或钼包套放入烧结炉中进行压力烧结,即得B4C基复合陶瓷材料。
5.根据权利要求4所述的制备方法,其特征在于:所述B4C粉末的粒度为0.5-5μm,纯度不低于96%;所述Ti3SiC2粉末的粒度为0.5-10μm,纯度不低于98%;所述金属氢化物粉末的粒度为0.5-10μm,纯度不低于98%。
6.根据权利要求4所述的制备方法,其特征在于:步骤2中,所述压力烧结为放电等离子烧结、热压烧结或热等静压烧结。
7.根据权利要求6所述的制备方法,其特征在于:
当采用放电等离子烧结时,烧结条件为:烧结炉真空状态下,对样品施加压力10MPa并加热升温至700℃保温10min,随后施加压力至30MPa,继续升温至烧结温度并保温,升温速率为50-100℃/min,烧结温度为1700-1800℃,保温时间为10-20min;保温结束后随即降压、降温,样品随炉冷却;
当采用热压烧结时,烧结条件为:烧结炉真空状态下,以5-20℃/min的升温速率将样品加热至1700-1850℃,保温时间为60-180min,加载压力为15-40MPa;保温结束后随即降压、降温,样品随炉冷却;
当采用热等静压烧结时,烧结条件为:在氩气下以30-100℃/min的升温速率将样品加热至1600-1800℃,保温时间为60-240min,加载压力为150-300MPa;保温结束后随即降压、降温,样品随炉冷却。
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