CN112830791A - 一种高熵陶瓷及其制备方法和应用 - Google Patents
一种高熵陶瓷及其制备方法和应用 Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 108
- 238000010438 heat treatment Methods 0.000 claims abstract description 43
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 36
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 22
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims abstract description 22
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000011812 mixed powder Substances 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 238000002490 spark plasma sintering Methods 0.000 claims abstract description 13
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000001681 protective effect Effects 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 238000000498 ball milling Methods 0.000 claims abstract description 11
- 238000011049 filling Methods 0.000 claims abstract description 10
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(IV) oxide Inorganic materials O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 9
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 9
- 238000001354 calcination Methods 0.000 claims abstract description 8
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 3
- 238000007723 die pressing method Methods 0.000 claims abstract description 3
- 229910052735 hafnium Inorganic materials 0.000 claims abstract description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 3
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 3
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 3
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 3
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 3
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 3
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 3
- 239000002245 particle Substances 0.000 claims description 54
- 229910002804 graphite Inorganic materials 0.000 claims description 16
- 239000010439 graphite Substances 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 8
- 239000003054 catalyst Substances 0.000 abstract 1
- 239000006104 solid solution Substances 0.000 description 30
- 239000012071 phase Substances 0.000 description 13
- 239000002994 raw material Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- CSJDCSCTVDEHRN-UHFFFAOYSA-N methane;molecular oxygen Chemical compound C.O=O CSJDCSCTVDEHRN-UHFFFAOYSA-N 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000003921 particle size analysis Methods 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
- 238000000713 high-energy ball milling Methods 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 229910003862 HfB2 Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 229910007948 ZrB2 Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
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Abstract
本发明属于陶瓷材料技术领域,公开了一种高熵陶瓷及其制备方法和应用。该高熵陶瓷分子式为(Me1aMe2bMe3cMe4dMe5eMe6fMe7gMe8h)B2,其中0.1≤a≤0.9,0.1≤b≤0.9,0.1≤c≤0.9,0.1≤d≤0.9,0.1≤e≤0.9,0.1≤f≤0.9,0≤g≤0.9,0≤h≤0.9且a+b+c+d+e+f+g+h=1;Me1‑Me8为Hf、Mo、Zr、Nb、Ti、V、W、Cr、Ta中的任意6~8种;该高熵陶瓷是将金属氧化物HfO2、MoO3、ZrO2、Nb2O5、TiO2、V2O5、WO3、Cr2O3、Ta2O5中的任意6~8种和B4C、碳粉加入溶剂经球磨混合得到混合粉体,经压模后所得坯体升温至1400~1600℃,采用放电等离子烧结将所得高熵粉体升温至1000~1400℃时充入保护气氛,然后升温至1900~2100℃,加压10~100MPa煅烧制得。高熵陶瓷的相对密度>98%,硬度为35~40GPa,热导率为0.1~1W/(mK)。
Description
技术领域
本发明属于陶瓷材料技术领域,更具体地,涉及一种高熵陶瓷及其制备方法和应用。
背景技术
“高熵”是近年来出现的新的材料设计理论,目前已成为材料研究领域的一大热点,其概念最初由高熵合金发展而来。高熵陶瓷是一种无机非金属材料,一般由4种以上的等比例或近等比例金属元素和若干种非金属元素结合而成的单相陶瓷材料。
高熵陶瓷具有高强度、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。由于组分的增加,用于探索和发现新材料的组合空间大大增加,但是大多数成分不会形成均一的单相。
高熵陶瓷由于组分的增加,陶瓷体系的构型熵增加,导致其吉布斯自由能下降,使得陶瓷体系更为稳定,性能表现出优异的稳定性。另外,由于各种原子随机分布在晶格点阵中,每个原子周围的环境以及占位均不一样,使得晶格内部有更多的晶格畸变和缺陷,滑移困难,性能提高。已报道文献中多为4元或5元的高熵陶瓷,6元及6元以上的高熵陶瓷少见报道。
发明内容
为了解决上述现有技术存在的不足和缺点,提供一种高熵陶瓷。该陶瓷具有超多组元,均一固溶体相、组元稳定、硬度高及热导率低的优点。
本发明另一目的在于提供上述高熵的陶瓷的制备方法。
本发明再一目的在于提供上述高熵的陶瓷的应用。
本发明的目的通过下述技术方案来实现:
一种高熵陶瓷,所述高熵陶瓷分子式为(Me1aMe2bMe3cMe4dMe5eMe6fMe7gMe8h)B2,其中0.1≤a≤0.9,0.1≤b≤0.9,0.1≤c≤0.9,0.1≤d≤0.9,0.1≤e≤0.9,0.1≤f≤0.9,0≤g≤0.9,0≤h≤0.9且a+b+c+d+e+f+g+h=1;Me1-Me8为Hf、Mo、Zr、Nb、Ti、V、W、Cr、Ta中的任意6~8种;该高熵陶瓷是将金属氧化物HfO2、MoO3、ZrO2、Nb2O5、TiO2、V2O5、WO3、Cr2O3、Ta2O5中的任意6~8种和B4C、碳粉加入溶剂经球磨混合得到混合粉体,经压模后所得坯体放入石墨坩埚中,升温至1400~1600℃保温,进行真空热处理得到高熵粉体;采用放电等离子烧结将高熵粉体升温至1000~1400℃时充入保护气氛,然后升温至1900~2100℃,加压10~100MPa煅烧制得。
优选地,所述a+b+c+d+e+f+g+h=1,且a、b、c、d、e、f、g和h为等摩尔。
优选地,所述金属氧化物的纯度为99.0~99.9wt%,金属氧化物的粒径为0.1~10μm;所述B4C粉和碳粉的纯度为97~99.99wt.%,粒径为1~2μm。
优选地,所述高熵粉体的纯度99.0~99.9wt%,粒径为0.1~1μm;所述高熵粉体的氧含量为0.01~0.1wt%,碳含量为0.01~0.5wt%。
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1400~1600℃的升温速率为5~15℃/min;所述保温时间为0.5~2h;所述升温至1000~1400℃的升温速率为100~400℃/min,所述升温至1900~2100℃时的升温速率为100~400℃/min。
优选地,所述陶瓷的相对密度>98%,硬度为35~40GPa,热导率为0.1~1W/(mK)。
所述的高熵陶瓷的制备方法,包括如下具体步骤:
S1.将金属氧化物HfO2、MoO3、ZrO2、Nb2O5、TiO2、V2O5、WO3、Cr2O3、Ta2O5中的任意6~8种和B4C、碳粉加入溶剂和球磨介质,在球磨机上混合10~48h,干燥后得混合粉体;
S2.将混合粉体模压后的坯体放入石墨坩埚中,以5~15℃/min的速率升温至1400~1600℃保温0.5~2h,真空热处理,获得(Me1aMe2bMe3cMe4dMe5eMe6fMe7gMe8h)B2高熵粉体;
S3.将(Me1aMe2bMe3cMe4dMe5eMe6fMe7gMe8h)B2高熵粉体放入石墨模具中,采用放电等离子烧结以100~400℃/min的速率升温至1000~1400℃并充入保护气氛,再以100~400℃/min的速率升温至1900~2100℃,保温10~30min,加压10~100MPa煅烧,制得(Me1aMe2bMe3cMe4dMe5eMe6fMe7gMe8h)B2高熵陶瓷。
所述的高熵陶瓷在高温核反应堆、航空航天领域中的应用。所述的高温为>2000℃,超硬(>35GPa)低热导率(<1W/(mK))。
本发明的高熵陶瓷是以6~8种氧化物为原料,经过硼热碳热还原反应,制备出(Me1aMe2bMe3cMe4dMe5eMe6fMe7gMe8h)B2高熵粉体,Me1、Me2、Me3、Me4、Me5、Me6、Me7、Me8金属间相互固溶,经放电等离子烧结后,由于其冷却速度快,很难出现固溶析出相,制备出单相的(Me1aMe2bMe3cMe4dMe5eMe6fMe7gMe8h)B2高熵陶瓷。其组分均一,性能稳定,且一种粉末具有多组元的性质。
与现有技术相比,本发明具有以下有益效果:
1.本发明的高熵陶瓷由于其具有6种或6种以上的组元,很难烧结出单相固溶体陶瓷,在高混合熵的条件下,材料的分相倾向性被抑制,仅出现简单的单一物相。相比于4元或者5元高熵陶瓷,组元更多,提高了高熵陶瓷的构型熵,使得体系吉布斯自由能降低,陶瓷性能更加稳定。
2.本发明通过固相反应制备出的高熵粉体,由于其粉末粒径小,纯度高,烧结驱动力大,易于烧出单相固溶体陶瓷。
3.本发明合成的高熵陶瓷粉末,相比于多种硼化物经高能球磨后获得的混合粉末,避免了高能球磨过程球磨介质的污染,从而降低高熵陶瓷粉末的污染,烧结出的高熵陶瓷性能更为优异,具有超硬(>35GPa)和低热导率(<1W/(mK))。
4.本发明的高熵陶瓷由于组元增多,各组元发生固溶,由于原子半径的差异,出现了大量的晶格畸变,其性能优于各单一组元材料,其具有更高的声子散射,相比于各组元陶瓷,拥有更低的热导率(0.1~1W/(mK))。
说明附图
图1为实施例1制得的(Hf1/6Mo1/6Zr1/6Nb1/6Ti1/6V1/6)B2高熵粉体和陶瓷的XRD图谱。
图2为实施例1制得的(Hf1/6Mo1/6Zr1/6Nb1/6Ti1/6V1/6)B2高熵陶瓷的断口形貌。
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(粉末的纯度99%,粒径1μm)、MoO3(粉末的纯度99%,粒径3μm)、ZrO2(粉末的纯度99.8%,粒径1μm)、Nb2O5(粉末的纯度99.8%,粒径5μm)、TiO2(粉末的纯度99%,粒径0.5μm)、V2O5(粉末的纯度99.6%,粒径1μm)和B4C(粉末的纯度99.9%,粒径0.5μm)、碳粉(粉末的纯度99%,粒径0.8μm)为原料,以乙醇为溶剂,以Si4N3为球磨介质,在球磨机上混合24h,干燥后得到混合粉体;
2.将混合粉体模压后的坯体放入石墨坩埚中,以10℃/min的速率升温至1600℃保温1h,真空热处理获得(Hf1/6Mo1/6Zr1/6Nb1/6Ti1/6V1/6)B2高熵粉体。
3.将(Hf1/6Mo1/6Zr1/6Nb1/6Ti1/6V1/6)B2高熵粉体放入石墨模具中,采用放电等离子烧结以150℃/min的速率升温至1000℃并充入Ar保护气氛,再以150℃/min的速率升温至2000℃,保温10min,加压30MPa煅烧,制得(Hf1/6Mo1/6Zr1/6Nb1/6Ti1/6V1/6)B2高熵陶瓷。
图1为实施例1制得的(Hf1/6Mo1/6Zr1/6Nb1/6Ti1/6V1/6)B2高熵粉体和陶瓷的XRD图谱。其中,(a)为(Hf1/6Mo1/6Zr1/6Nb1/6Ti1/6V1/6)B2高熵陶瓷粉末,(b)为(Hf1/6Mo1/6Zr1/6Nb1/6Ti1/ 6V1/6)B2高熵陶瓷。从图1中可以看出,本实例制得的(Hf1/6Mo1/6Zr1/6Nb1/6Ti1/6V1/6)B2高熵陶瓷粉末中没有检测到HfO2、MoO3、ZrO2、Nb2O5、TiO2、V2O5相,只有(Hf1/6Mo1/6Zr1/6Nb1/6Ti1/6V1/6)B2高熵陶瓷粉末相和少量未固溶的HfB2相。与HfB2标准PDF卡片65-8678和ZrB2标准PDF卡片65-8704对比可知,(Hf1/6Mo1/6Zr1/6Nb1/6Ti1/6V1/6)B2的峰向高角度偏移,高熵固熔体为均一的固熔体相,说明高熵固熔体粉末经过SPS烧结后仍为均一的固熔体相。图2为本实例经SPS烧结后(Hf1/6Mo1/6Zr1/6Nb1/6Ti1/6V1/6)B2高熵陶瓷的断口形貌,从图2可以看出,所制得的高熵陶瓷比较致密,只存在少量气孔,实现了高熵陶瓷的致密化烧结。
通过激光粒度分析测得本实施例固溶体粉末的粉末粒径为0.39μm,用碳氧分析仪测得固溶体粉末的含氧量为0.01wt%,固溶体粉末的碳含量为0.03wt%,制备得到的具有多元高熵的陶瓷材料形成单一的固溶体,其相对密度为98%,硬度为35GPa,热导率为0.3W/(mK)。
实施例2
1.以HfO2(粉末的纯度99%,粒径1μm)、MoO3(粉末的纯度99%,粒径3μm)、ZrO2(粉末的纯度99.8%,粒径1μm)、Nb2O5(粉末的纯度99.8%,粒径5μm)、TiO2(粉末的纯度99%,粒径0.5μm)、WO3(粉末的纯度99.5%,粒径4μm)和B4C(粉末的纯度99.9%,粒径0.5μm)、碳粉(粉末的纯度99%,粒径0.8μm)为原料,以乙醇为溶剂,以Si4N3为球磨介质,在球磨机上混合24h,干燥后得到混合粉体;
2.将混合粉体模压后的坯体放入石墨坩埚中,以15℃/min的速率升温至1400℃保温1h,真空热处理获得(Hf1/6Mo1/6Zr1/6Nb1/6Ti1/6W1/6)B2高熵粉体。
3.将(Hf1/6Mo1/6Zr1/6Nb1/6Ti1/6W1/6)B2高熵粉体放入石墨模具中,采用放电等离子烧结以200℃/min的速率升温至1400℃并充入Ar保护气氛,再以200℃/min的速率升温至2100℃,保温30min,加压45MPa煅烧,制得(Hf1/6Mo1/6Zr1/6Nb1/6Ti1/6W1/6)B2高熵陶瓷。
通过激光粒度分析测得本实施例固溶体粉末的粉末粒径为0.62μm,用碳氧分析仪测得固溶体粉末的含氧量为0.02wt%,固溶体粉末的碳含量为0.02wt%,制备得到的具有多元高熵的陶瓷材料形成单一的固溶体,其相对密度为98%,硬度为35GPa,热导率为0.6W/(mK)。
实施例3
1.以HfO2(粉末的纯度99%,粒径1μm)、MoO3(粉末的纯度99%,粒径3μm)、ZrO2(粉末的纯度99.8%,粒径1μm)、Nb2O5(粉末的纯度99.8%,粒径5μm)、TiO2(粉末的纯度99%,粒径0.5μm)、Cr2O3(粉末的纯度99.5%,粒径3μm)和B4C(粉末的纯度99.9%,粒径0.5μm)、碳粉(粉末的纯度99%,粒径0.8μm)为原料,以乙醇为溶剂,以Si4N3为球磨介质,在球磨机上混合24h,干燥后得到混合粉体;
2.将混合粉体模压后的坯体放入石墨坩埚中,以5℃/min的速率升温至1500℃保温2h,真空热处理获得(Hf1/6Mo1/6Zr1/6Nb1/6Ti1/6Cr1/6)B2高熵粉体。
3.将(Hf1/6Mo1/6Zr1/6Nb1/6Ti1/6Cr1/6)B2高熵粉体放入石墨模具中,采用放电等离子烧结以300℃/min的速率升温至1200℃并充入Ar保护气氛,再以100℃/min的速率升温至2000℃保温20min,加压50MPa煅烧,制得(Hf1/6Mo1/6Zr1/6Nb1/6Ti1/6Cr1/6)B2高熵陶瓷。
通过激光粒度分析测得本实施例固溶体粉末的粉末粒径为0.39μm,用碳氧分析仪测得固溶体粉末的含氧量为0.01wt%,固溶体粉末的碳含量为0.03wt%,制备得到的具有多元高熵的陶瓷材料形成单一的固溶体,其相对密度为98%,硬度为36GPa,热导率为0.5W/(mK)。
实施例4
1.以HfO2(粉末的纯度99%,粒径1μm)、MoO3(粉末的纯度99%,粒径3μm)、ZrO2(粉末的纯度99.8%,粒径1μm)、Nb2O5(粉末的纯度99.8%,粒径5μm)、TiO2(粉末的纯度99%,粒径0.5μm)、V2O5(粉末的纯度99.6%,粒径1μm)、WO3(粉末的纯度99.5%,粒径4μm)和B4C(粉末的纯度99.9%,粒径0.5μm)、碳粉(粉末的纯度99%,粒径0.8μm)为原料,以乙醇为溶剂,以Si4N3为球磨介质,在球磨机上混合24h,干燥后得到混合粉体;
2.将混合粉体模压后的坯体放入石墨坩埚中,以10℃/min的速率升温至1500℃保温0.5h,真空热处理获得(Hf1/7Mo1/7Zr1/7Nb1/7Ti1/7V1/7W1/7)B2高熵粉体。
3.将(Hf1/7Mo1/7Zr1/7Nb1/7Ti1/7V1/7W1/7)B2高熵粉体放入石墨模具中,采用放电等离子烧结以150℃/min的速率升温至1200℃并充入Ar保护气氛,再以150℃/min的速率升温至1950℃,保温15min,加压35MPa煅烧,制得(Hf1/7Mo1/7Zr1/7Nb1/7Ti1/7V1/7W1/7)B2高熵陶瓷。
通过激光粒度分析测得本实施例固溶体粉末的粉末粒径为0.26μm,用碳氧分析仪测得固溶体粉末的含氧量为0.01wt%,固溶体粉末的碳含量为0.06wt%,制备得到的具有多元高熵的陶瓷材料形成单一的固溶体,其相对密度为99%,硬度为40GPa,热导率为0.4W/(mK)。
实施例5
1.以HfO2(粉末的纯度99%,粒径1μm)、MoO3(粉末的纯度99%,粒径3μm)、ZrO2(粉末的纯度99.8%,粒径1μm)、Nb2O5(粉末的纯度99.8%,粒径5μm)、TiO2(粉末的纯度99%,粒径0.5μm)、Ta2O5(粉末的纯度99.6%,粒径1μm)、WO3(粉末的纯度99.5%,粒径4μm)和B4C(粉末的纯度99.9%,粒径0.5μm)、碳粉(粉末的纯度99%,粒径0.8μm)为原料,以乙醇为溶剂,以Si4N3为球磨介质,在球磨机上混合24h,干燥后得到混合粉体;
2.将混合粉体模压后的坯体放入石墨坩埚中,以15℃/min的速率升温至1400℃保温1h,真空热处理获得(Hf1/7Mo1/7Zr1/7Nb1/7Ti1/7Ta1/7W1/7)B2高熵粉体。
3.将(Hf1/7Mo1/7Zr1/7Nb1/7Ti1/7Ta1/7W1/7)B2高熵粉体放入石墨模具中,采用放电等离子烧结以250℃/min的速率升温至1000℃并充入Ar保护气氛,再以150℃/min的速率升温至1900℃,保温10min,加压20MPa煅烧,制得(Hf1/7Mo1/7Zr1/7Nb1/7Ti1/7Ta1/7W1/7)B2高熵陶瓷。
通过激光粒度分析测得本实施例固溶体粉末的粉末粒径为0.23μm,用碳氧分析仪测得固溶体粉末的含氧量为0.01wt%,固溶体粉末的碳含量为0.07wt%,制备得到的具有多元高熵的陶瓷材料形成单一的固溶体,其相对密度为99%,硬度为39GPa,热导率为0.8W/(mK)。
本发明合成的高熵陶瓷粉末,相比于多种硼化物经高能球磨后获得的混合粉末,避免了高能球磨过程球磨介质的污染,从而降低高熵陶瓷粉末的污染,烧结出的高熵陶瓷性能更为优异,所述陶瓷的相对密度>98%,硬度为35~40GPa,热导率为0.1~1W/(mK)。
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)
1.一种高熵陶瓷,其特征在于,所述高熵陶瓷分子式为(Me1aMe2bMe3cMe4dMe5eMe6fMe7gMe8h)B2,其中0.1≤a≤0.9,0.1≤b≤0.9,0.1≤c≤0.9,0.1≤d≤0.9,0.1≤e≤0.9,0.1≤f≤0.9,0≤g≤0.9,0≤h≤0.9且a+b+c+d+e+f+g+h=1;Me1-Me8为Hf、Mo、Zr、Nb、Ti、V、W、Cr、Ta中的任意6~8种;该高熵陶瓷是将金属氧化物HfO2、MoO3、ZrO2、Nb2O5、TiO2、V2O5、WO3、Cr2O3、Ta2O5中的任意6~8种和B4C、碳粉加入溶剂经球磨混合得到混合粉体,经压模后所得坯体放入石墨坩埚中,升温至1400~1600℃保温,进行真空热处理得到高熵粉体;采用放电等离子烧结将高熵粉体升温至1000~1400℃时充入保护气氛,然后升温至1900~2100℃,加压10~100MPa煅烧制得。
2.根据权利要求1所述的高熵陶瓷,其特征在于,所述a+b+c+d+e+f+g+h=1,且a、b、c、d、e、f、g和h为等摩尔。
3.根据权利要求1所述的高熵陶瓷,其特征在于,所述金属氧化物的纯度为99.0~99.9wt%,金属氧化物的粒径为0.1~10μm;所述B4C粉和碳粉的纯度为97~99.99wt.%,其粒径为1~2μm。
4.根据权利要求1所述的高熵陶瓷,其特征在于,所述高熵粉体的纯度99.0~99.9wt%,粒径为0.1~1μm;所述高熵粉体的氧含量为0.01~0.1wt%,碳含量为0.01~0.5wt%。
5.根据权利要求1所述高熵陶瓷,其特征在于,所述溶剂为乙醇、丙醇、甲醇或丙酮。
6.根据权利要求1所述的高熵陶瓷,其特征在于,所述保护气氛为N2或Ar。
7.根据权利要求1所述的高熵陶瓷,其特征在于,所述升温至1400~1600℃的升温速率为5~15℃/min;所述保温时间为0.5~2h;所述升温至1000~1400℃的升温速率为100~400℃/min;所述升温至1900~2100℃时的升温速率为100~400℃/min。
8.根据权利要求1所述的高熵陶瓷,其特征在于,所述陶瓷的相对密度>98%,硬度为35~40GPa,热导率为0.1~1W/(mK)。
9.根据权利要求1-8任一项所述的高熵陶瓷的制备方法,其特征在于,包括如下具体步骤:
S1.将金属氧化物HfO2、MoO3、ZrO2、Nb2O5、TiO2、V2O5、WO3、Cr2O3、Ta2O5中的任意6~8种和B4C、碳粉加入溶剂和球磨介质,在球磨机上混合10~48h,干燥后得混合粉体;
S2.将混合粉体模压后的坯体放入石墨坩埚中,以5~15℃/min的速率升温至1400~1600℃保温0.5~2h,真空热处理,获得(Me1aMe2bMe3cMe4dMe5eMe6fMe7gMe8h)B2高熵粉体;
S3.将(Me1aMe2bMe3cMe4dMe5eMe6fMe7gMe8h)B2高熵粉体放入石墨模具中,采用放电等离子烧结以100~400℃/min的速率升温至1000~1400℃并充入保护气氛,再以100~400℃/min的速率升温至1900~2100℃,保温10~30min,加压10~100MPa煅烧,制得(Me1aMe2bMe3cMe4dMe5eMe6fMe7gMe8h)B2高熵陶瓷。
10.权利要求1~8任一项所述的高熵陶瓷在高温核反应堆、航空航天领域中的应用。
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