CN109516811B - 一种具有多元高熵的陶瓷及其制备方法和应用 - Google Patents
一种具有多元高熵的陶瓷及其制备方法和应用 Download PDFInfo
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Abstract
本发明属于陶瓷材料技术领域,公开了一种具有多元高熵的陶瓷及其制备方法和应用。该陶瓷是以Me1的氧化物、Me2的氧化物、Me3的氧化物、Me4的氧化物、Me5的氧化物和无定型硼粉为原料,球磨混合后压制成坯体;放入石墨坩埚中进行真空热处理得(Me1xMe2yMe3zMe4nMe5m)B2固熔体粉体;采用放电等离子烧结将上述固熔体粉体升温至1000~1400℃时充入保护气氛,然后升温至1800~2200℃煅烧制得。所得多元高熵陶瓷的相对密度>95%,硬度为25~35GPa,断裂韧性为2~8MPa·m1/2,晶粒尺寸为0.1~1.1μm,经1000℃~1500℃热处理后重量变化率为0.3~1%。
Description
技术领域
本发明属于表面功能薄膜材料技术领域,更具体地,涉及一种具有多元高熵的陶瓷及其制备方法和应用。
背景技术
随着航空、航天、电子、通信等技术以及机械、化工、能源等工业的发展,对材料的性能提出越来越高、越来越多的要求,传统的单一材料已不能满足使用要求。高熵陶瓷具有五种或五种以上的组元,若其固溶成为单相固熔体陶瓷,因具有较高的熵值,易获得热稳定性高的固溶相和纳米结构,不同的高熵陶瓷具有不同的特性,其表现优于传统陶瓷材料。多组元高熵陶瓷是一个可合成、可加工、可分析、可应用的新陶瓷世界,具有很高的学术研究价值和很大的工业发展潜力。
阻碍陶瓷向多元方向发展的主要原因是:传统陶瓷的发展经验告诉我们,虽然可以通过添加特定的少量陶瓷元素来改善性能,但元素种类过多会导致很多化合物尤其是脆性金属间化合物的出现,从而导致陶瓷性能的恶化,如变脆等。此外,也给材料的组织和成分分析带来很大困难。难熔金属的硼化物,ZrB2、HfB2、 NbB2、TaB2、CrB2、TiB2和MoB2因其优异的物理、化学和机械性能而备受关注。其多组元高熵陶瓷也具有高强度、硬度、优异的耐磨性、优异的耐高温强度、良好的结构稳定性和良好的耐蚀性和抗氧化性。其制备均使用商业购买的硼化物粉体,高能球磨后烧结出陶瓷材料,但是只有少量的报道成功制备出单相高熵陶瓷,因此关于这些材料及其特性还有很多需要研究的地方。
发明内容
为了解决上述现有技术存在的不足和缺点,提供一种具有多元高熵的陶瓷。该陶瓷具有均一固溶体相的、组元稳定的、力学性能及抗氧化性能优异的高熵陶瓷。
本发明另一目的在于提供上述具有多元高熵陶瓷的制备方法。
本发明再一目的在于提供上述具有多元高熵陶瓷的应用。
本发明的目的通过下述技术方案来实现:
一种具有多元高熵的陶瓷,所述陶瓷是以Me1的氧化物、Me2的氧化物、Me3的氧化物、Me4的氧化物、Me5的氧化物和无定型硼粉为原料,加入溶剂经球磨混合得混合粉体,经模压后所得坯体放入石墨坩埚中,升温至800~1200℃保温Ⅰ后,再升温至1400~1600℃保温Ⅱ,进行真空热处理得(Me1x Me2yMe3zMe4nMe5m)B2固熔体粉体;采用放电等离子烧结将(Me1x Me2yMe3zMe4nMe5m)B2固熔体粉体升温至1000~1400℃时充入保护气氛,然后升温至1800~2200℃煅烧制得;所述0.1≤x≤0.9,0.1≤y≤0.9,0.1≤z≤0.9,0.1≤n≤0.9,0.1≤m≤0.9。
优选地,x=0.2,y=0.2,z=0.2,n=0.2,m=0.2。
优选地,所述陶瓷的相对密度>95%,硬度为25~35GPa,断裂韧性 2~8MPa·m1/2,晶粒尺寸为0.1~1.1μm,所述陶瓷在1000~1500℃热处理后重量变化率为0.3~1%。
优选地,所述固熔体粉体(Me1xMe2yMe3zMe4nMe5m)B2的纯度 99.0-99.9wt%,所述固熔体粉体的粒径为0.1~1μm,所述固熔体粉体的氧含量为 0.1-0.5wt%,所述固熔体粉体的碳含量为0.1~0.5wt%。
优选地,所述固熔体粉体(Me1x Me2yMe3zMe4nMe5m)B2中Me1、Me2、 Me3、Me4和Me5为Hf、Zr、Ti、Nb、Ta、Mo或Cr。
优选地,所述溶剂为乙醇、丙醇、甲醇或丙酮。
优选地,所述保护气氛为N2或Ar。
优选地,所述升温至800~1200℃和升温至1400~1600℃时的速率均为 5~20℃/min,所述保温Ⅰ和保温Ⅱ的时间均为0.5~2h;所述煅烧的时间为1~30min,所述煅烧的压力为10~100MPa,所述升温至1800~2200℃时的升温的速率为 100~400℃/min。
所述的具有多元高熵的陶瓷的制备方法,包括如下具体步骤:
S1.以Me1的氧化物、Me2的氧化物、Me3的氧化物、Me4的氧化物、Me5 的氧化物和无定型硼粉为原料,加入溶剂和球磨介质,在球磨机上混合10~48h,干燥后获得混合粉体;
S2.将混合粉体模压后的坯体放入石墨坩埚中,以5~20℃/min的速率升温至800~1200℃保温0.5~2h,然后再以5~20℃/min的速率升温至1400~1600℃保温0.5~2h,获得(Me1x Me2yMe3zMe4nMe5m)B2固熔体粉体;
S3.将(Me1x Me2yMe3zMe4nMe5m)B2固熔体粉体放入石墨模具中,采用放电等离子烧结以100~400℃/min速率升温至1000~1400℃时充保护气氛,再以 100~400℃/min速率升温至1800~2200℃,保温1~30min,加压10~100MPa煅烧,制得(Me1xMe2yMe3zMe4nMe5m)B2多元高熵的陶瓷。
所述具有多元高熵的陶瓷在超高温抗氧化器件领域中的应用。
本发明的一种具有多元高熵的陶瓷,所述陶瓷是将单相固熔体粉体(Me1xMe2yMe3zMe4nMe5m)B2为原料,Me1,Me2,Me3,Me4,Me5五元金属之间固溶,经过放电等离子烧结后,由于其冷却速度快,很难出现固溶析出相,获得的陶瓷仍为(Me12Me22Me32Me42Me52)B2单相多元高熵的陶瓷体,组分均一,成分稳定,性能优异,且一种粉末具有多元金属的性质。
与现有技术相比,本发明具有以下有益效果:
1.本发明采用固相法自合成的超细高熵陶瓷粉末,通过放电等离子烧结制备多元高熵陶瓷材料,研究表明此固相法合成的高熵陶瓷粉末晶粒较细,且组分均一。晶粒尺寸小,成分均匀的原料粉末,且烧结出的高熵陶瓷材料性能优异。
2.本发明的方法反应原料就为单相固熔体粉末,相比于多种硼化物高能球磨获得的混合原料粉末物理上均匀性,该方法达到了原料组分的化学均匀性。这也有利于其烧结材料的均匀固熔体相的形成,也节约能源与成本。
3.本发明的方法制备的高熵陶瓷材料,由于原料是固熔体粉末,形成固熔体可以促进原子扩散,可在低温下实现烧结致密,改善烧结性能,提高材料性能。
4.本发明的方法采用SPS实现高熵陶瓷材料的快速制备,极大缩短了晶粒长大时间,可获得晶粒细小的陶瓷,原料粉体成本低且原料粉末相对于商业购买的硼化物粉末细,其在烧结过程中扩散较快,更易烧结出单相高熵陶瓷材料,这会使得高熵陶瓷材料的组织更细小,更大的提高材料的性能。
附图说明
图1为实施例中2制得的(Hf0.2Mo0.2Ta0.2Nb0.2Ti0.2)B2高熵固熔体粉末的 XRD图。
图2为实施例2中制得经SPS烧结后(Hf0.2Mo0.2Ta0.2Nb0.2Ti0.2)B2高熵陶瓷的XRD图。
具体实施方式
下面结合具体实施例进一步说明本发明的内容,但不应理解为对本发明的限制。若未特别指明,实施例中所用的技术手段为本领域技术人员所熟知的常规手段。除非特别说明,本发明采用的试剂、方法和设备为本技术领域常规试剂、方法和设备。
实施例1
1.以HfO2、ZrO2、Nb2O5、Ta2O5和Cr2O3和无定型硼粉为原料,以乙醇为溶剂,以Si3N4球为球磨介质,在球磨机上混合,干燥后获得混合粉体;
2.将混合粉体模压后获得坯体放入石墨坩埚中,以10℃/min的速率升温至 1200℃保温1h,然后再以10℃/min的速率升温至1600℃保温1h,真空热处理后的获得(Hf0.2Zr0.2Nb0.2Ta0.2Cr0.2)B2超细高熵陶瓷固熔体粉末。
3.将(Hf0.2Zr0.2Nb0.2Ta0.2Cr0.2)B2多元高熵固熔体粉末为原料粉体,将其放入石墨模具中,以300℃/min升温速率将温度升至2000℃,保温5min,加压80MPa,在1200℃时充Ar气,通过放电等离子(SPS)烧结,制得具有多元高熵的陶瓷材料。
通过激光粒度分析测得本实施例多元高熵的陶瓷固熔体粉末的粒径为 0.34μm,用碳氧分析仪测得固熔体粉末的氧含量为0.1wt%,固熔体粉末的碳含量为0.02wt%。制备得到的具有多元高熵的陶瓷材料形成了均一的单相固熔体。其相对密度为99%,硬度30GPa,断裂韧性6MPa·m1/2,晶粒尺寸为0.50μm,陶瓷的抗氧化性能良好,1200℃热处理后重量增加了0.85%。
实施例2
1.以HfO2、MoO3、Nb2O5、Ta2O5和TiO2和无定型硼粉为原料,以乙醇为溶剂,以Si3N4球为球磨介质,在球磨机上混合,干燥后获得混合粉体;
2.将混合粉体模压后获得坯体放入石墨坩埚中,以10℃/min的速率升温至 1100℃保温1h,然后再以10℃/min的速率升温至1550℃保温1h,真空热处理后获得(Hf0.2Mo0.2Ta0.2Nb0.2Ti0.2)B2超细高熵固熔体粉末。
3.将(Hf0.2Mo0.2Ta0.2Nb0.2Ti0.2)B2多元高熵固熔体粉末放入石墨模具中,以200℃/min升温速率将温度升至1800℃,保温5min,加压40MPa,1200℃时充 Ar气,通过放电等离子烧结获得多元高熵陶瓷材料。
图1为本实施例制得的(Hf0.2Mo0.2Ta0.2Nb0.2Ti0.2)B2高熵固熔体粉末的XRD 图。其中,(a)为氧化物混合粉末,(b)为(Hf0.2Mo0.2Ta0.2Nb0.2Ti0.2)B2多元高熵固熔体粉末,从图1中可知氧化物混合粉末中存在HfO2、Ta2O5、Nb2O5、 TiO2的和MoO3相,(Hf0.2Mo0.2Ta0.2Nb0.2Ti0.2)B2固熔体粉末只有一相,说明氧化物混合粉末经过热处理后,Hf,Mo,Ta,Nb和Ti之间发生固溶,形成了单相多元高熵固溶体粉末;
图2为本实施例制得的经SPS烧结后(Hf0.2Mo0.2Ta0.2Nb0.2Ti0.2)B2高熵陶瓷的XRD图。其中,(a)为(Hf0.2Mo0.2Ta0.2Nb0.2Ti0.2)B2多元高熵固熔体粉末; (b)为(Hf0.2Mo0.2Ta0.2Nb0.2Ti0.2)B2多元高熵陶瓷。从图2中可知, (Hf0.2Mo0.2Ta0.2Nb0.2Ti0.2)B2多元高熵固熔体粉末中只有一相,与HfB2标准PDF 卡片65-86778对比可知,(Hf0.2Mo0.2Ta0.2Nb0.2Ti0.2)B2的峰向高角度偏移,多元高熵固熔体粉末为均一的固熔体相。说明多元高熵固熔体粉末经过SPS烧结后仍为均一的固熔体相。
通过激光粒度分析测得本实施例固熔体粉末的粒径为0.10μm,用碳氧分析仪测得固熔体粉末的氧含量为0.08wt%,固熔体粉末的碳含量为0.01wt%,制备得到的具有多元高熵的陶瓷材料形成了均一的单相固熔体,其相对密度为99%,硬度35GPa,断裂韧性5MPa·m1/2,晶粒尺寸为0.10μm,陶瓷的抗氧化性能良好,1200℃热处理后重量增加了0.35%。
实施例3
1.以HfO2、ZrO2、Nb2O5、MoO3和Cr2O3和无定型硼粉为原料,以乙醇为溶剂,以Si3N4球为球磨介质,在球磨机上混合,干燥后获得混合粉体;
2.将混合粉体模压后获得坯体放入石墨坩埚中,以10℃/min的速率升温至1000℃保温1h,然后再以10℃/min的速率升温至1550℃保温1h,真空热处理后的获得(Hf0.2Zr0.2Nb0.2Mo0.2Cr0.2)B2超细高熵固熔体粉末;
3.将(Hf0.2Zr0.2Nb0.2Mo0.2Cr0.2)B2多元高熵固熔体粉末放入石墨模具中,以100℃/min升温速率将温度升至2000℃,保温30min,加压10MPa,1200℃时充Ar气,通过放电等离子烧结,制得具有多元高熵的陶瓷材料。
通过激光粒度分析测得本实施例固熔体粉末的粒径为0.80μm,用碳氧分析仪测得固熔体粉末的氧含量为0.01wt%,固熔体粉末的碳含量为0.03wt%,制备得到的具有多元高熵的陶瓷材料形成了均一的单相固熔体,其相对密度为99%,硬度25GPa,断裂韧性8MPa·m1/2,晶粒尺寸为1.10μm,陶瓷的抗氧化性能良好,1200℃热处理后重量增加了0.71%。
实施例4
1.以HfO2、TiO2、Nb2O5、Ta2O5和Cr2O3和无定型硼粉为原料,以乙醇为溶剂,以Si3N4球为球磨介质,在球磨机上混合,干燥后获得混合粉体;
2.将混合粉体模压后获得坯体放入石墨坩埚中,以10℃/min的速率升温至 1200℃保温1h,然后再以10℃/min的速率升温至1550℃保温1h,真空热处理后的获得(Hf0.2Ti0.2Nb0.2Ta0.2Cr0.2)B2超细高熵陶瓷固溶体粉末。
3.将(Hf0.2Ti0.2Nb0.2Ta0.2Cr0.2)B2多元高熵陶瓷粉末放入石墨模具中,以150℃/min升温速率将温度升至2000℃,保温15min,加压50MPa,1200℃时充 Ar气,通过放电等离子烧结,制得具有多元高熵的陶瓷材料。
通过激光粒度分析测得本实施例固熔体粉末的粒径为0.39μm,用碳氧分析仪测得固熔体粉末的氧含量为0.15wt%,固溶体粉末的碳含量为0.01wt%,制备得到的具有多元高熵的固熔体材料形成了均一的单相固熔体,其相对密度为99%,硬度30GPa,断裂韧性4.23MPa·m1/2,晶粒尺寸为0.45μm,陶瓷的抗氧化性能良好,1400℃热处理后重量增加了0.72%。
实施例5
1.以HfO2、TiO2、ZrO2、Ta2O5和Cr2O3和无定型硼粉为原料,以乙醇为溶剂,以Si3N4球为球磨介质,在球磨机上混合,干燥后获得混合粉体;
2.将混合粉体模压后获得坯体放入石墨坩埚中,以10℃/min的速率升温至 1150℃保温1h,然后再以10℃/min的速率升温至1550℃保温1h,真空热处理后的获得(Hf0.2Zr0.2Ti0.2Ta0.2Cr0.2)B2超细高熵陶瓷固熔体粉末。
3.将(Hf0.2Ti0.2Nb0.2Ta0.2Cr0.2)B2多元高熵陶瓷粉末放入石墨模具中,以 400℃/min升温速率将温度升至2000℃,保温1min,加压100MPa,1200℃时充Ar 气,通过放电等离子烧结,制得具有多元高熵的陶瓷材料。
通过激光粒度分析测得本实施例固溶体粉末的粒径为0.39μm,用碳氧分析仪测得固熔体粉末的氧含量为0.13wt%,固熔体粉末的碳含量为0.02wt%,制备得到的具有多元高熵的陶瓷材料形成了均一的单相固熔体,其相对密度为99%,硬度35GPa,断裂韧性6MPa·m1/2,晶粒尺寸为0.52μm,陶瓷的抗氧化性能良好,1500℃热处理后重量增加了0.3%。
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、组合和简化,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)
1.一种具有多元高熵的陶瓷,其特征在于,所述陶瓷是以Me1的氧化物、Me2的氧化物、Me3的氧化物、Me4的氧化物、Me5的氧化物和无定型硼粉为原料,加入溶剂经球磨混合得混合粉体,经模压后所得坯体放入石墨坩埚中,升温至800~1200℃保温Ⅰ后,再升温至1400~1600℃保温Ⅱ,进行真空热处理得(Me1x Me2yMe3zMe4nMe5m)B2固熔体粉体;采用放电等离子烧结将(Me1x Me2yMe3zMe4nMe5m)B2固熔体粉体升温至1000~1400℃时充入保护气氛,然后升温至1800~2200℃煅烧制得;所述0.1≤x≤0.9,0.1≤y≤0.9,0.1≤z≤0.9,0.1≤n≤0.9,0.1≤m≤0.9;所述陶瓷的晶粒尺寸为0.1~1.1μm。
2.根据权利要求1所述的具有多元高熵的陶瓷,其特征在于,所述x=0.2,y=0.2,z=0.2,n=0.2,m=0.2。
3.根据权利要求1所述的具有多元高熵的陶瓷,其特征在于,所述陶瓷的相对密度>95%,硬度为25~35GPa,断裂韧性2~8MPa·m1/2,所述陶瓷在1000~1500℃热处理后重量变化率为0.3~1%。
4.根据权利要求1所述的具有多元高熵的陶瓷,其特征在于,所述固熔体粉体(Me1xMe2yMe3zMe4nMe5m)B2的纯度99.0~99.9wt%,所述固熔体粉体的粒径为0.1~1μm,所述固熔体粉体的氧含量为0.1~0.5wt%,所述固熔体粉体的碳含量为0.1~0.5wt%。
5.根据权利要求1所述的具有多元高熵的陶瓷,其特征在于,所述固熔体粉体(Me1xMe2yMe3zMe4nMe5m)B2中Me1、Me2、Me3、Me4和Me5为Hf、Zr、Ti、Nb、Ta、Mo或Cr。
6.根据权利要求1所述的具有多元高熵的陶瓷,其特征在于,所述溶剂为乙醇、丙醇、甲醇或丙酮。
7.根据权利要求1所述的具有多元高熵的陶瓷,其特征在于,所述保护气氛为N2或Ar。
8.根据权利要求1所述的具有多元高熵的陶瓷,其特征在于,所述升温至800~1200℃和升温至1400~1600℃时的速率均为5~20℃/min,所述保温Ⅰ和保温Ⅱ的时间均为0.5~2h;所述煅烧的时间为1~30min,所述煅烧的压力为10~100MPa,所述升温至1800~2200℃时的升温的速率为100~400℃/min。
9.根据权利要求1-8任一项所述的具有多元高熵的陶瓷的制备方法,其特征在于,包括如下具体步骤:
S1.以Me1的氧化物、Me2的氧化物、Me3的氧化物、Me4的氧化物、Me5的氧化物和无定型硼粉为原料,加入溶剂和球磨介质,在球磨机上混合10~48h,干燥后获得混合粉体;
S2.将混合粉体模压后的坯体放入石墨坩埚中,以5~20℃/min的速率升温至800~1200℃保温0.5~2h,然后再以5~20℃/min的速率升温至1400~1600℃保温0.5~2h,进行真空热处理获得(Me1x Me2yMe3zMe4nMe5m)B2固熔体粉体;
S3.将(Me1x Me2yMe3zMe4nMe5m)B2固熔体粉体放入石墨模具中,采用放电等离子烧结以100~400℃/min速率升温至1000~1400℃时充保护气氛,再以100~400℃/min速率升温至1800~2200℃,保温1~30min,加压10~100MPa煅烧,制得(Me1x Me2yMe3zMe4nMe5m)B2多元高熵的陶瓷。
10.权利1~8任一项所述具有多元高熵的陶瓷在超高温抗氧化器件领域中的应用。
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