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High Quality YBa2Cu3O7-x Superconducting Thin Films Grown by MOCVD MOCVD生长高质量YBa2Cu3O7-x超导薄膜
Pub Date : 1995-06-01 DOI: 10.1051/JPHYSCOL:1995543
C. Dubourdieu, J. Sénateur, O. Thomas, F. Weiss
YBCO thin films have been grown by Metal Organic Chemical Vapour Deposition in a cold wall type reactor. The β-diketonates of yttrium, barium and copper are used as precursors. Films have been deposited on (001) MgO and (012) LaAlO 3 single crystalline substrates. The morphology is very dependant on the gas phase composition. Different oxygen partial pressures have been investigated. An increasing oxygen partial pressure - at a fixed deposition temperature - is found to increase the growth rate and to promote the growth of a-axis grains (grains with the c axis parallel to the substrate's surface). In our standard deposition conditions, Ti subs t rate holder = 875°C, P Total = 5 Torr, and P O2 = 2 Torr, high quality films are obtained, exhibiting T C ∼ 91 K (10%-90% of the resistive transition) and J C (77K) ∼ 5.10 6 A/cm 2 . A trilayer structure YBCO/Y 2 O 3 /YBCO (900A/100A/900A) has been grown on LaAlO 3 substrate, with the epitaxial relationship: (001) YBCO // or (001) Y2O3 . No misorientations have been found in the (a,b) plane. The trilayer exhibits a sharp superconducting transition (ΔT C = 0.4 K), with T C = 82.5 K, and J C (77 K) ∼ 10 6 A/cm 2 .
采用金属有机化学气相沉积法在冷壁反应器中制备了YBCO薄膜。钇、钡和铜的β-二酮酸盐用作前体。薄膜沉积在(001)MgO和(012)LaAlO 3单晶衬底上。形貌与气相组成有很大关系。研究了不同的氧分压。在固定的沉积温度下,增加氧分压可以提高生长速度,促进a轴晶粒(c轴平行于衬底表面的晶粒)的生长。在我们的标准沉积条件下,Ti subt rate holder = 875°C, P Total = 5 Torr, P O2 = 2 Torr,获得了高质量的薄膜,表现出t C ~ 91 K(10%-90%的电阻转变)和J C (77K) ~ 5.10 6 A/ cm2。在LaAlO 3衬底上生长出了YBCO/ Y2O3 /YBCO (900A/100A/900A)三层结构,外延关系为(001)YBCO/ /或(001)Y2O3。在(a,b)平面上没有发现定向错误。三层材料表现出明显的超导跃迁(ΔT C = 0.4 K),温度为82.5 K,温度为77 K ~ 10.6 a / cm2。
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引用次数: 4
Mass Flow Controlled Evaporation System 质量流量控制蒸发系统
Pub Date : 1995-06-01 DOI: 10.1051/JPHYSCOL:19955113
H. Boer
In many (CVD-) processes, there is an increasing demand for delivering reactants as near liquid vapours. Controlling vapours, however, is often a delicate matter. The proven method is the well known bubbler system, with it's inherent problems: poor stability and poor reproducibility, due to the extremely high sensitivity for changes in temperature. The system described in this paper is an evaporation system, based on mass flow controllers. The vapour is controlled in the liquid phase; thus the amount of vapour is controlled, stable and reproducible, independent of temperature or pressure. Special attention is given to the new possibilities that come into reach with this system, e.g. fluids with very low vapour pressures which are unstable at high temperatures and mixtures can be evaporated properly in this system.
在许多(CVD-)过程中,以接近液态蒸汽的形式输送反应物的需求越来越大。然而,控制蒸汽通常是一件微妙的事情。经过验证的方法是众所周知的起泡器系统,其固有的问题是:稳定性差,可重复性差,由于对温度变化的敏感性极高。本文所描述的系统是一个基于质量流量控制器的蒸发系统。蒸汽控制在液相中;因此,水蒸气的量是可控的、稳定的和可重复的,不受温度或压力的影响。特别要注意的是,该系统可以达到新的可能性,例如,在高温下不稳定的蒸气压非常低的流体和混合物可以在该系统中适当地蒸发。
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引用次数: 19
Simulation of Epitaxial Silicon Chemical Vapor Deposition in Barrel Reactors 外延硅化学气相沉积在桶状反应器中的模拟
Pub Date : 1995-06-01 DOI: 10.1051/JPHYSCOL:1995530
M. Masi, S. Fogliani, S. Carrà
The epitaxial silicon chemical vapor deposition by SiCl 4 /H 2 mixtures in a LPE 861 barrel reactor has been simulated by means of a detailed 2D model solved by the commercial finite element code FIDAP. Different reactor configurations (i.e., bell diameter, gas diffusors, susceptor tilting angle) and deposition conditions (i.e., flow rates and reactor pressure) have been examined. The simulation have been satisfactorily compared with experimental growth rate data measured along the reactor axial coordinate.
本文采用商用有限元软件FIDAP对sicl4 / h2混合物在LPE 861桶状反应器中外延硅化学气相沉积过程进行了详细的二维模型模拟。研究了不同的反应器结构(即钟型直径、气体扩散器、导流器倾斜角)和沉积条件(即流速和反应器压力)。模拟结果与沿反应器轴向坐标测量的实验生长速率数据进行了比较,结果令人满意。
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引用次数: 0
Volatile Metals Coordination Compounds as Precursors for Functional Materials Synthesis by CVD-Method 挥发性金属配位化合物作为cvd法合成功能材料的前驱体
Pub Date : 1995-06-01 DOI: 10.1051/JPHYSCOL:1995564
E. Mazurenko, A. I. Gerasimchuk
The applications of such coordination compounds (chelates) as metal β-diketonates in different CVD techniques were examined. It was shown that high chemical and physical characteristics of these compounds allow their favourable use comparatively with other volatile compounds. The general miles in volatility and thermal stability of β-diketonates and their fluorine derivatives were discussed. The ways of preparation of various functional materials with specific properties were determined.
考察了金属β-二酮酸酯等配合物在不同化学气相沉积技术中的应用。结果表明,与其他挥发性化合物相比,这些化合物具有较高的化学和物理特性。讨论了β-二酮酸酯及其氟衍生物的挥发性和热稳定性。确定了各种具有特定性能的功能材料的制备方法。
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引用次数: 1
Mass Spectrometric Study of Thermolysis Mechanism of Metal Acetylacetonates Vapour 金属乙酰丙酮酸蒸气热裂解机理的质谱研究
Pub Date : 1995-06-01 DOI: 10.1051/JPHYSCOL:1995521
A. Bykov, A. E. Turgambaeva, I. Igumenov, P. P. Semyannikov
The processes of thermal decomposition of aluminium(III) and scandium(III) acetylacetonates (Al(aa) 3 and Sc(aa) 3 ) were investigated in the 160-650°C temperature range using a high-temperature molecular beam source with mass spectrometric sampling of the gas phase composition directly at the outlet from the reaction zone. A scheme of thermal decomposition of aluminium(III) and scandium(III) acetylacetonates vapour is suggested. It is established that the common mechanism of thermolysis of these complexes is due to the commonness of electronic structure of ions Mg 2+ , Al 3+ , Sc 3+ and Hf 4+ . According to the scheme, the process proceeds along three parallel routes, one of them being possible only for complexes possessing more than two ligands, in this case the gaseous products resulting from cyclic dimerization of ligand fragments are formed. The influence of oxygen and hydrogen on the composition of the gaseous products and the mechanism of thermolysis of the complexes vapour are also established. From temperature curves, the effective values of kinetic parameters in Arrhenius equation are calculated for the first order reaction.
采用高温分子束源,在160 ~ 650℃的温度范围内,研究了乙酰丙酮酸铝(III)和乙酰丙酮酸钪(Al(aa) 3和Sc(aa) 3)的热分解过程,并对反应区出口气相组成进行了质谱采样。提出了乙酰丙酮酸铝(III)和乙酰丙酮酸钪(III)蒸气的热分解方案。确定了这些配合物的共同热裂解机理是由于Mg 2+、Al 3+、Sc 3+和Hf 4+离子具有共同的电子结构。根据该方案,该过程沿着三条平行路线进行,其中一条路线仅适用于具有两个以上配体的配合物,在这种情况下,由配体片段的循环二聚化产生的气体产物形成。建立了氧和氢对气态产物组成的影响以及配合物蒸汽的热分解机理。根据温度曲线,计算了一级反应的动力学参数有效值。
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引用次数: 8
Deposition of MoO3 Films from a Volatile Molybdenyl Complex 挥发性钼基配合物沉积MoO3薄膜
Pub Date : 1995-06-01 DOI: 10.1051/JPHYSCOL:1995559
B. Ballarin, E. Brescacin, G. Rizzi, E. Tondello
A volatile molybdenyl complex was used as precursor for MOCVD of MoO 3 films. Decomposition paths were investigated by thermal analysis. Good quality films were obtained on different substrates and characterized by XPS, UV-Vis, XRD and SEM analyses. The different electronic properties of the various films on different substrates were studied by photoemission experiments and compared with respect to the MoO 3 single crystal.
采用挥发性钼基配合物作为moo3薄膜MOCVD的前驱体。通过热分析研究了分解路径。采用XPS、UV-Vis、XRD和SEM等方法对不同的衬底制备的薄膜进行了表征。通过光电发射实验研究了不同衬底上不同薄膜的不同电子性能,并与moo3单晶进行了比较。
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引用次数: 0
Remote microwave plasma enhanced chemical vapour deposition of SiO2 films: oxygen plasma diagnostic 远程微波等离子体增强SiO2薄膜化学气相沉积:氧等离子体诊断
Pub Date : 1995-06-01 DOI: 10.1051/JPHYSCOL:1995574
C. Regnier, J. Desmaison, P. Tristant, D. Merle
Silicon oxide is deposited by remote microwave plasma enhanced chemical vapour deposition (RMPECVD). The silica films are produced by exciting oxygen in a microwave discharge while a mixture of 5% of silane diluted in argon is introduced downstream. In the afterglow, double Langmuir probe measurements and rotational temperatures deduced from optical emission spectroscopy (OES), show that the electron energy is transferred to the gas when the pressure increases (19 - 26 Pa). Therefore the electronic temperature decreases from 22000 to 11000 K and the gas temperature increases from 400 to 500 K. Moreover the microwave power (180 -480 W) has an influence on the deposition rate and on the quality of SiO 2 coatings (density and etch rate in an HF solution). This effect can be correlated with the increase in the electron density (0.7.10 10 to 3.7.10 10 cm -3 ) and of the gas temperature (400 to 460 K).
采用微波等离子体增强化学气相沉积(RMPECVD)技术制备氧化硅。在微波放电中激发氧气制备二氧化硅薄膜,同时在下游引入5%硅烷在氩气中稀释的混合物。在余辉中,双朗缪尔探针测量和从光学发射光谱(OES)推断的旋转温度表明,当压力增加(19 - 26 Pa)时,电子能量转移到气体中。因此电子温度从22000 K下降到11000 K,气体温度从400 K上升到500 K。此外,微波功率(180 -480 W)对沉积速率和sio2涂层质量(在HF溶液中的密度和蚀刻速率)也有影响。这种效应与电子密度(0.7.10 - 10 ~ 3.7.10 - 10 cm -3)和气体温度(400 ~ 460 K)的增加有关。
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引用次数: 4
Modelling of Precursor Flow and Deposition in Atomic Layer Deposition Reactor 原子层沉积反应器中前驱体流动与沉积的模拟
Pub Date : 1995-06-01 DOI: 10.1051/JPHYSCOL:1995528
H. Siimon, J. Aarik
A calculation model to study atomic layer deposition (ALD) in low-pressure channel-type CVD reactor with many parallel substrates is described. The calculations are based on continuity equation and kinetic equation for surface coverage. Formation of a steady-state adsorption wave propagating between the substrates during a precursor pulse is studied. The effect of diffusion and sticking coefficients, carrier gas flow rate and growth temperature on formation and propagation of the steady-state adsorption wave is analyzed.
建立了一种用于研究具有多个平行衬底的低压通道型CVD反应器中原子层沉积(ALD)的计算模型。计算基于表面覆盖度的连续性方程和动力学方程。研究了在前驱体脉冲中在衬底间传播的稳态吸附波的形成。分析了扩散系数和黏附系数、载气流速和生长温度对稳态吸附波形成和传播的影响。
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引用次数: 7
Deposition of Platinum from Bis(Acetylacetonato)Platinum(II) 双(乙酰丙酮)铂沉积铂(II)
Pub Date : 1995-06-01 DOI: 10.1051/JPHYSCOL:1995512
J. Arndt, L. Klippe, R. Stolle, G. Wahl
The evaporation and deposition process of Bis(acetylacetonato)platinum(II) (Pt(acac) 2 ) was examined in a computerized microbalance system, which allows the measuring of the mass of evaporating precursor and depositing layer simultaneously. The investigations were carried out in an argon-atmosphere and an argon/oxygen-atmosphere with pressure ranging from 250 Pa to 1000 Pa. The deposition kinetics were investigated in the temperature range between T dep = 523 K and T dep = 733 K. A strong dependence of the deposition rate on the pretreatment of the substrate was observed. Beginning the deposition on alumina with low deposition temperatures T dep an activation energy of 204 ± 9 kJ/mol was found. On platinum precoated substrates we observed higher deposition rates and lower values for the activation energy, if the precoating was carried out at temperature T pre > T dep . At long deposition times with T dep = const. the deposition rates on precoated substrates decreased to the values obtained without precoating at higher temperatures. This effect has not been clarified. In argon-atmosphere platinum layers containing carbon were deposited. Increasing the deposition temperature caused increased carbon contamination. The carbon can be removed by oxidation in air after the deposition. Platinum coatings without carbon contamination were obtained by adding oxygen during the deposition process.
在微机微平衡系统中研究了双(乙酰丙酮)铂(II) (Pt(acac) 2)的蒸发和沉积过程,该系统可以同时测量蒸发前驱体和沉积层的质量。研究在氩气气氛和氩气/氧气氛中进行,压力范围为250 ~ 1000 Pa。在T深度= 523 ~ 733 K的温度范围内研究了沉积动力学。观察到沉积速率与基底预处理有很强的依赖性。在较低的沉积温度下,在氧化铝上开始沉积,发现活化能为204±9 kJ/mol。在铂预涂基底上,我们观察到如果在温度T预> T深度进行预涂,则沉积速率更高,活化能值更低。在较长的沉积时间下,T深度= const。在较高温度下,预涂基板上的沉积速率降低到没有预涂的值。这种影响尚未得到澄清。在氩气氛中沉积了含碳铂层。升高沉积温度导致碳污染增加。沉积后的碳可以在空气中氧化去除。在沉积过程中加入氧气,得到了无碳污染的铂镀层。
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引用次数: 8
Refractory Coatings of C-Me-Si and C-Me-B-Si Systems for Protection of Carbon Materials (CM) 碳材料防护用C-Me-Si和C-Me-B-Si体系耐火涂料
Pub Date : 1995-06-01 DOI: 10.1051/JPHYSCOL:1995597
S. G. Andryushin, A. Kasatkin
The three-zoned structure of the coatings for protection from high-temperature oxidation of carbon materials (CM) was grounded. The kinetic of formation and phase composition of diffusion coating C-Me-Si and C-Me-B-Si (Me = Ti, Zr or Hf) systems formed on CM (graphite and carbon/carbon materials) have been studied. The coating on CM received by using sequential metallization, boron- and silicium- deposition from dispersive solid-phased media. The rate of formation coatings of C-Me-Si by metallization and Si-deposition on CM decreases on the line: Ti--Zr--Hf, and the formation carbide layers MeC by diffusion metallization CM describes linear-parabolic law have been shown. The velocity of boron diffusion of the CM - MeC layer compositions is very little and it is increased on the line: Ti--Zr--Hf insignificantly. The formation of MeB 2 layer at the boriding are decreased of the velocity of siliciding. The coating proposed base three-zoned structure formed by compounds of C-Me-Si or C-Me-B-Si systems and intended for protection of CM from high-temperature oxidation (T>1400°C). The laws of phase form and destruction at high-temperature oxidation in air for these coatings are investigated.
对碳材料高温氧化防护涂层的三带结构进行了研究。研究了在CM(石墨和碳/碳材料)上形成的C-Me-Si和C-Me-B-Si (Me = Ti, Zr或Hf)扩散涂层体系的形成动力学和相组成。在分散固相介质中采用顺序金属化、硼和硅沉积的方法在CM上获得涂层。金属化和硅沉积在CM上形成C-Me-Si涂层的速率在Ti—Zr—Hf线上呈递减趋势,而扩散金属化CM在MeC上形成碳化物层符合线性—抛物线规律。CM - MeC层成分中硼的扩散速度很小,在Ti—Zr—Hf线上硼的扩散速度增加不显著。硼化过程中meb2层的形成随着硅化速度的增加而减少。该涂层提出了由C- me - si或C- me - b - si体系化合物形成的碱性三带结构,用于保护CM免受高温氧化(T>1400°C)。研究了这些涂层在空气中高温氧化时的相形成和破坏规律。
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引用次数: 0
期刊
Le Journal De Physique Colloques
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