CN109678504A - 一种二价镁离子掺杂钽酸钇高温陶瓷及其制备方法 - Google Patents
一种二价镁离子掺杂钽酸钇高温陶瓷及其制备方法 Download PDFInfo
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- 229910052727 yttrium Inorganic materials 0.000 title claims abstract description 34
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000011214 refractory ceramic Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000000498 ball milling Methods 0.000 claims abstract description 20
- 150000002500 ions Chemical class 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000007873 sieving Methods 0.000 claims abstract description 6
- 239000011812 mixed powder Substances 0.000 claims abstract description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 14
- 239000000395 magnesium oxide Substances 0.000 claims description 11
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims description 8
- 229910001936 tantalum oxide Inorganic materials 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 7
- 150000002910 rare earth metals Chemical class 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 5
- 238000005245 sintering Methods 0.000 claims description 5
- 230000003647 oxidation Effects 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 2
- 238000003701 mechanical milling Methods 0.000 claims description 2
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 6
- 229960000935 dehydrated alcohol Drugs 0.000 abstract description 6
- 239000003963 antioxidant agent Substances 0.000 abstract description 5
- 230000003078 antioxidant effect Effects 0.000 abstract description 5
- 235000006708 antioxidants Nutrition 0.000 abstract description 5
- NYWITVDHYCKDAU-UHFFFAOYSA-N oxygen(2-) yttrium(3+) zirconium(4+) Chemical compound [O--].[O--].[Y+3].[Zr+4] NYWITVDHYCKDAU-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract 2
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 238000007789 sealing Methods 0.000 abstract 1
- 239000011777 magnesium Substances 0.000 description 36
- 238000000748 compression moulding Methods 0.000 description 10
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 9
- 230000007423 decrease Effects 0.000 description 8
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 238000000280 densification Methods 0.000 description 5
- 238000000227 grinding Methods 0.000 description 5
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 5
- 238000010008 shearing Methods 0.000 description 5
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 description 5
- 229910001928 zirconium oxide Inorganic materials 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 239000012720 thermal barrier coating Substances 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- -1 rare earth aluminate Chemical class 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 229910002080 8 mol% Y2O3 fully stabilized ZrO2 Inorganic materials 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical group [F-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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- C04B35/495—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
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Abstract
本发明公开一种二价镁离子掺杂钽酸钇高温陶瓷及其制备方法，属于高温陶瓷制备技术领域。本发明所述Mg2+离子掺杂钽酸钇高温陶瓷的结构式为Y1‑xMgxTaO(4‑x/2)（x为0~0.16)；通过化学式Y1‑xMgxTaO(4‑x/2)计算可以按比例称量氧化物原料，将称量好的原料和无水乙醇一起放置在球磨罐中混合、密封后置于行星式球磨机上球磨，使其能够混合均匀，将混合后的粉末干燥、过筛后，置于模具内压实，然后在高温炉中进行烧结。本发明工艺简单，通过Mg2+离子掺杂钽酸钇，产品热导低，热膨胀系数较高，接近氧化钇稳定性氧化锆(7%‑8%YSZ)的热膨胀系数，并且制备成本低，适合批量生产，目的产品有望作为新型低热导，抗氧化，耐高温陶瓷材料。
Description
技术领域
本发明涉及一种二价镁离子掺杂钽酸钇高温陶瓷及其制备方法，属于高温陶瓷制备技术领域。
背景技术
从近些年对高温陶瓷材料的发展来看，可能适用于高温热障涂层的陶瓷材料主要有氧化钇/氧化铈稳定的氧化锆、氧化锆/氧化铝、稀土锆酸盐，稀土铝酸盐，稀土磷酸盐，多元氧化物稳定氧化锆，稀土焦绿石或萤石结构化合物，磷灰石结构稀土硅酸盐石榴石（YAG）结构，磁铅石结构，钙钛矿结构等材料，由于氧化钇稳定的氧化锆（YSZ）具备优良的综合性能，因此是目前广泛应用的陶瓷热障涂层。但是氧化钇稳定的氧化锆（YSZ）在温度超过1200℃，会存在一定的缺陷，首先是高温相稳定性，氧化钇稳定的氧化锆（YSZ）是以一种亚稳态四方相（t’）存在，在较高温度下（>1200 ℃时），会转变为四方相（t）和立方相（c）的混合物；其次，YSZ的烧结速率会随温度升高而加快，研究表明在YSZ涂层的制备过程中会产生微量的SiO2杂质，而SiO2杂质的存在将显著提高YSZ涂层高温下的烧结速率，导致气孔率减小，从而使热导率升高，最终将导致热障涂层陶瓷材料脱落失效，已经难以满足热能发动机前燃气进口温度不断提高的要求。因此，亟需寻求一种能够长期稳定工作于1200℃以上条件下的新型热障涂层陶瓷材料。
发明内容
本发明的目的在于提供一种二价镁离子掺杂钽酸钇高温陶瓷，主要用于热障涂层材料，有很好的热学及力学性能，其结构式为Y1-xMgxTaO(4-x/2)（x为 0~0.16)。
本发明的另一目的在于提供所述二价镁离子掺杂钽酸钇高温陶瓷的制备方法，具体包括以下步骤：
（1）按照Mg2+掺杂量的不同称取相应的氧化镁、氧化钽和稀土氧化钇，通过球磨的方法混合均匀；
（2）混匀之后的样品经过干燥、过筛，将过筛后的粉末置于模具内压实，然后在高温炉中进行烧结，得到Mg2+离子掺杂钽酸钇高温陶瓷。
优选的，本发明步骤（1）中球磨过程中球磨机的转速为400~500r/min，球磨时间为160~200min。
优选的，本发明步骤（2）中干燥过程的温度为70~80℃，时间为12~24小时；过筛过程中粉末过250~350目筛。
优选的，本发明步骤（2）中混合粉末压实时，保压压力为10~15MPa，保压时间为20~40min。
优选的，本发明步骤（2）中在高温炉中烧结温度为1650~1700 ℃，煅烧时间为10~12小时。
本发明所述氧化镁、氧化钽和稀土氧化钇的纯度≥ 99.99%。
本发明的有益效果是：
（1）本发明所述方法中粉末能够完全混合均匀，在烧结过程中完全反应，所制得的二价Mg2+离子掺杂钽酸钇高温陶瓷有很好的高温热稳定性，有望作为一种潜在的高温陶瓷材料。
（2）所制得的二价Mg2+离子掺杂钽酸钇高温陶瓷在高温下热导较低1.45～1.65 W/mk，在高温下热膨胀系数为（（9～9.5）×10–6 K -1）。
附图说明
图1为实施例4制备的（Y0.84Mg0.16TaO3.92）高温陶瓷块体的扫描电镜图 (SEM图谱)。
图2为实施例4制备的（Y0.84Mg0.16TaO3.92）与氧化钇稳定性氧化锆 (7%-8%YSZ) 的热导率的图谱。
具体实施方式
下面结合具体实施方式对本发明进行详细说明，但本发明的保护范围并不限于所述内容。
实施例1
一种钽酸钇高温陶瓷材料（YTaO4）的制备方法，具体包括以下步骤：
称取氧化钇2.825g，氧化钽5.525g，在无水乙醇中混合，置于行星式球磨机中球磨（球磨机的转速为400 r/min，球磨时间为180min），将球磨好的混合物在74℃下干燥24小时后过300目筛，然后用模具压制成型（保压压力为10 MPa，保压时间为30 min），压制成型后，将其在1700℃下煅烧10小时，冷却至室温，即得到所需致密的钽酸钇高温陶瓷（YTaO4）高温陶瓷，反应方程式为Y2O3 + Ta2O5 = 2YTaO4。
如表1所示，本实施例制备得到的钽酸钇高温陶瓷材料的体模量、杨氏模量和剪切模量的值分别为：130.7, 148.7，52.4Gpa；根据Clarke和Slack模型，以及公式、求出Y1-xMgxTaO(4-x/2)（x为 0~0.16)陶瓷的极限热导率；从Clarke模型可以得出体模量对于热导有着重要的影响，其模量越低，热导越低，使得改陶瓷材料能应用在绝热材料方面的可能性；从Slack模型我们可以得知，德拜温度对于热导也是一个重要的参数，如果德拜温度越低，其热导也越低；可见这些热性能参数都是影响热导的重要因数；在力学方面，其纯样品的硬度大约为5.15Gpa。
实施例2
一种耐高温、抗氧化、抗磨损二价Mg2+离子掺杂钽酸钇高温陶瓷材料（Y0.96Mg0.04TaO3.98）的制备方法，具体包括以下步骤：
称取氧化镁0.04g，氧化钇2.712g，氧化钽5.525g，在无水乙醇中混合后，置于行星式球磨机中球磨（球磨机的转速为400 r/min，球磨时间为180min），将球磨好的混合物在74 ℃下干燥24小时后过300目筛，然后用模具压制成型（保压压力为10 MPa，保压时间为30min），压制成型后，将其在1700℃下煅烧10小时，冷却至室温，即得到所需致密的二价Mg2+离子掺杂钽酸钇高温陶瓷（Y0.96Mg0.04TaO3.98）高温陶瓷，反应方程式为0.04 MgO + 0.48 Y2O3 + 0.5 Ta2O5 = Y0.96Mg0.04TaO3.98。
如表1所示，本实施例制备得到的Y0.96Mg0.04TaO3.98的体模量、杨氏模量和剪切模量的值分别为98.1，145.5，60.4Gpa；Y0.96Mg0.04TaO3.98相对于纯样品杨氏模量的值有所下降，并且德拜温度的值也有明显的下降；所以根据Clarke和Slack模型算出来的热导相对于纯样品的热导有所降低；其硬度相对于纯样有所下降，其维氏硬度值大约为：5.03Gpa。
实施例3
一种耐高温、抗氧化、抗磨损二价Mg2+离子掺杂钽酸钇高温陶瓷材料（Y0.92Mg0.08TaO3.96）的制备方法，具体包括以下步骤：
称取氧化镁0.08g，氧化钇2.599g，氧化钽5.525g，在无水乙醇中混合后，置于行星式球磨机中球磨（球磨机的转速为400 r/min，球磨时间为180min），将球磨好的混合物在74 ℃下干燥24小时后过300目筛，然后用模具压制成型（保压压力为10 MPa，保压时间为30min），压制成型后，将其在1700℃下煅烧10小时，冷却至室温，即得到所需致密的二价Mg2+离子掺杂钽酸钇高温陶瓷（Y0.92Mg0.08TaO3.96）高温陶瓷，反应方程式为0.08 MgO + 0.46 Y2O3 + 0.5 Ta2O5 = Y0.92Mg0.08TaO3.96。
如表1所示，本实施例制备的Y0.92Mg0.08TaO3.96的体模量、杨氏模量和剪切模量的值分别为98.8，140.9，57.7Gpa；相对于纯样品和掺杂量为0.04g镁相比可以看出杨氏模量的值有所下降，并且德拜温度的值也有明显的下降；所以根据Clarke和Slack模型算出来的热导相对于纯样品的热导有所降低；其硬度相对于纯样有所下降，其维氏硬度值大约为：4.81Gpa。
实施例4
一种耐高温、抗氧化、抗磨损二价Mg2+离子掺杂钽酸钇高温陶瓷材料（Y0.88Mg0.12TaO3.94）的制备方法，具体包括以下步骤：
称取氧化镁0.12g，氧化钇2.486g，氧化钽5.525g，在无水乙醇中混合后，置于行星式球磨机中球磨（球磨机的转速为400 r/min，球磨时间为180min），将球磨好的混合物在74 ℃下干燥24小时后过300目筛，然后用模具压制成型（保压压力为15 MPa，保压时间为20min），压制成型后，将其在1700℃下煅烧10小时，冷却至室温，即得到所需致密的二价Mg2+离子掺杂钽酸钇高温陶瓷（Y0.88Mg0.12TaO3.94）高温陶瓷，反应方程式为0.12 MgO + 0.44 Y2O3 +0.5 Ta2O5 = Y0.88Mg0.12TaO3.94。
如表1所示，本实施例制备的Y0.88Mg0.12TaO3.94的体模量、杨氏模量和剪切模量的值分别为118.6，123.2，46.4Gpa；相对于纯样品和掺杂量为0.08g镁相比可以看出杨氏模量的值有所下降，并且德拜温度的值也有明显的下降；所以根据Clarke和Slack模型算出来的热导相对于纯样品的热导有所降低；其硬度相对于纯样有所下降，其维氏硬度值大约为：4.94Gpa。
实施例5
一种耐高温、抗氧化、抗磨损二价Mg2+离子掺杂钽酸钇高温陶瓷材料（Y0.84Mg0.16TaO3.92）的制备方法，具体包括以下步骤：
称取氧化镁0.16g，氧化钇2.373g，氧化钽5.525g，在无水乙醇中混合后，置于行星式球磨机中球磨（球磨机的转速为400 r/min，球磨时间为180min），将球磨好的混合物在74 ℃下干燥24小时后过300目筛，然后用模具压制成型（保压压力为10 MPa，保压时间为30min），压制成型后，将其在1700℃下煅烧10小时，冷却至室温，即得到所需致密的二价Mg2+离子掺杂钽酸钇高温陶瓷（Y0.84Mg0.16TaO3.92）高温陶瓷，反应方程式为0.16 MgO + 0.42 Y2O3 + 0.5 Ta2O5 = Y0.84Mg0.16TaO3.92。
如表1所示，本实施例制备的Y0.84Mg0.16TaO3.92的体模量、杨氏模量和剪切模量的值分别为86.1，94.9，36.1Gpa；相对于纯样品和掺杂量为0.12g镁相比可以看出杨氏模量的值有所下降，并且德拜温度的值也有明显的下降；所以根据Clarke和Slack模型算出来的热导相对于纯样品的热导有所降低；其硬度相对于纯样有所下降，其维氏硬度值大约为：4.86Gpa。
本实施例制备得到的二价Mg2+离子掺杂钽酸钇高温陶瓷（Y0.84Mg0.16TaO3.92）纯度高，形貌好，颗粒较细小，具有良好的性能，如图1所示的SEM图谱。如图2所示，本实验所制得的（Y0.84Mg0.16TaO3.92）与当前使用的7YSZ和8YSZ (2～3.5 W.m-1k-1)相比较，（Y0.84Mg0.16TaO3.92）在高温下有较低的热导率，根据高温热障涂层在使用情况下要具备的性能包括：熔点高、热导率低、热膨胀系数较高、耐高温氧化性较好、高温化学稳定性较好，与热生成氧化物氧化铝化学相容；（Y0.84Mg0.16TaO3.92）在高温下具备优良的热学性质以及力学性能；在力学方面，较低的硬度值（495 HV）可以有效地阻止残余应力和裂纹的传播，提高高温热障涂层的容韧性和断裂韧性，通过测试样品的模量可以对硬度值进行验证，并且（Y0.84Mg0.16TaO3.92）在高温下经试验测得热膨胀系数为约为9.5×10–6 K -1。因此二价Mg2+离子掺杂量为0.16g的钽酸钇高温陶瓷有很好的高温热稳定性，有望作为一种潜在的高温陶瓷材料。
表1：Y1-xMgxTaO(4-x/2)陶瓷的模量，硬度，德拜温度
。
Claims (6)
1.一种二价镁离子掺杂钽酸钇高温陶瓷，其特征在于：其结构式为Y1-xMgxTaO(4-x/2)（x为0~0.16)。
2.权利要求1所述二价镁离子掺杂钽酸钇高温陶瓷的制备方法，其特征在于，具体包括以下步骤：
（1）按照Mg2+掺杂量的不同称取相应的氧化镁、氧化钽和稀土氧化钇，通过球磨的方法混合均匀；
（2）混匀之后的样品经过干燥、过筛，将过筛后的粉末置于模具内压实，然后在高温炉中进行烧结，得到Mg2+离子掺杂钽酸钇高温陶瓷。
3.根据权利要求2所述二价镁离子掺杂钽酸钇高温陶瓷的制备方法，其特征在于：步骤（1）中球磨过程中球磨机的转速为400~500r/min，球磨时间为160~200min。
4.根据权利要求2所述二价镁离子掺杂钽酸钇高温陶瓷的制备方法，其特征在于：步骤（2）中干燥过程的温度为70~80℃，时间为12~24小时；过筛过程中粉末过250~350目筛。
5.根据权利要求2所述二价镁离子掺杂钽酸钇高温陶瓷的制备方法，其特征在于：步骤（2）中混合粉末压实时，保压压力为10~15MPa，保压时间为20~40min。
6.根据权利要求2所述二价镁离子掺杂钽酸钇高温陶瓷的制备方法，其特征在于：步骤（2）中在高温炉中烧结温度为1650~1700 ℃，煅烧时间为10~12小时。
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