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首页> 美国卫生研究院文献>Scientific Reports >Comparison of chemical stability and corrosion resistance of group IV metal oxide films formed by thermal and plasma-enhanced atomic layer deposition
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Comparison of chemical stability and corrosion resistance of group IV metal oxide films formed by thermal and plasma-enhanced atomic layer deposition

机译：通过热和等离子体增强原子层沉积形成的IV组金属氧化物膜的化学稳定性和耐腐蚀性的比较

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The wide applications of ultrathin group IV metal oxide films (TiO2, ZrO2 and HfO2) probably expose materials to potentially reactive etchants and solvents, appealing for extraordinary chemical stability and corrosion resistance property. In this paper, TiO2 ultrathin films were deposited on Si at 200 °C while ZrO2 and HfO2 were grown at 250 °C to fit their growth temperature window, by thermal atomic layer deposition (TALD) and plasma-enhanced ALD (PEALD). A variety of chemical liquid media including 1 mol/L H2SO4, 1 mol/L HCl, 1 mol/L KOH, 1 mol/L KCl, and 18 MΩ deionized water were used to test and compare chemical stability of all these as-deposited group IV metal oxides thin films, as well as post-annealed samples at various temperatures. Among these metal oxides, TALD/PEALD HfO2 ultrathin films exhibit the best chemical stability and anti-corrosion property without any change in thickness after long time immersion into acidic, alkaline and neutral solutions. As-deposited TALD ZrO2 ultrathin films have slow etch rate of 1.06 nm/day in 1 mol/L HCl, however other PEALD ZrO2 ultrathin films and annealed TALD ones show better anti-acid stability, indicating the role of introduction of plasma O2 in PEALD and post-thermal treatment. As-deposited TiO2 ultrathin films by TALD and PEALD are found to be etched slowly in acidic solutions, but the PEALD can decrease the etching rate of TiO2 by ~41%. After post-annealing, TiO2 ultrathin films have satisfactory corrosion resistance, which is ascribed to the crystallization transition from amorphous to anatase phase and the formation of 5% Si-doped TiO2 ultrathin layers on sample surfaces, i.e. Ti-silicate. ZrO2, and TiO2 ultrathin films show excellent corrosion endurance property in basic and neutral solutions. Simultaneously, 304 stainless steel coated with PEALD-HfO2 is found to have a lower corrosion rate than that with TALD-HfO2 by means of electrochemical measurement. The pre-treatment of plasma H2 to 304 stainless steel can effectively reduce interfacial impurities and porosity of overlayers with significantly enhanced corrosion endurance. Above all, the chemical stability and anti-corrosion properties of IV group metal oxide coatings can be improved by using PEALD technique, post-annealing process and plasma H2 pre-treatment to substrates.
机译：IV型超薄金属氧化物膜（TiO2，ZrO2和HfO2）的广泛应用可能会使材料暴露于潜在的反应性蚀刻剂和溶剂中，从而具有非凡的化学稳定性和耐腐蚀性。在本文中，通过热原子层沉积（TALD）和等离子体增强ALD（PEALD），在200°C的Si上沉积了TiO2超薄薄膜，而在250°C的ZrO2和HfO2上生长以适应其生长温度窗口。使用各种化学液体介质，包括1lmol / L的H2SO4、1lmol / L的HCl，1lmol / L的KOH，1lmol / L的KCl和18MΩ的去离子水来测试和比较所有这些沉积的化学稳定性IV族金属氧化物薄膜，以及在不同温度下的后退火样品。在这些金属氧化物中，TALD / PEALD HfO2超薄膜表现出最佳的化学稳定性和抗腐蚀性能，长时间浸泡在酸性，碱性和中性溶液中后厚度不变。沉积的TALD ZrO2超薄膜在1 mol / L HCl中的蚀刻速率慢，为1.06 nm / day，但是其他PEALD ZrO2超薄膜和退火的TALD膜显示出更好的抗酸稳定性，表明在PEALD中引入等离子体O2的作用和后热处理。发现TALD和PEALD沉积的TiO2超薄膜在酸性溶液中被缓慢腐蚀，但是PEALD可以使TiO2的腐蚀速率降低约41％。后退火后，TiO 2超薄膜具有令人满意的耐腐蚀性，这归因于从非晶相到锐钛矿相的结晶转变以及在样品表面即钛硅酸盐上形成了5％的Si掺杂的TiO 2超薄层。 ZrO 2 和TiO 2 超薄膜在碱性和中性溶液中均具有优异的耐腐蚀性能。同时，通过电化学测量发现，涂覆有PEALD-HfO 2 的304不锈钢的腐蚀速率低于TALD-HfO 2 的腐蚀速率。等离子体H 2 在304不锈钢上的预处理可以有效地降低界面杂质和覆盖层的孔隙率，并显着提高耐蚀性。最重要的是，通过使用PEALD技术，后退火工艺和等离子体H 2 预处理，可以改善IV族金属氧化物涂层的化学稳定性和防腐性能。

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