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Economical Analysis and Optimization of a Low Pressure Chemical Vapor Depositioni (LPCVD) Reactor 低压化学气相沉积(LPCVD)反应器的经济性分析与优化
Pub Date : 1995-06-01 DOI: 10.1051/JPHYSCOL:1995538
T. Tamani, P. Duverneuil, J. Couderc
An economical analysis of the LPCVD hot wall tubular reactor functioning is presented including equipment amortization, clean room location, supplies, maintenance, labor, gas and energy consumption. From a technical point of view, CVDI model is used to characterise the phenomena involved during polysilicon deposition, linking growth rate distribution to operating conditions. An optimization is then realized in three different cases with and without a temperature profile. By this study the main costs of CVD operation such as gases consumption and equipment amortization are identified, and the total cost has been drastically reduced by using a temperature profile.
对LPCVD热壁管式反应器的运行进行了经济分析,包括设备分期、洁净室选址、耗材、维护、人工、燃气和能源消耗等。从技术角度来看,CVDI模型用于表征多晶硅沉积过程中涉及的现象,将生长速率分布与操作条件联系起来。然后在有温度分布和没有温度分布的三种不同情况下实现优化。通过这项研究,确定了CVD操作的主要成本,如气体消耗和设备摊销,并通过使用温度剖面大大降低了总成本。
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引用次数: 0
MOCVD Routes to Tl2Ba2Can-1CunO4+2nSuperconductor and Dielectric Insulator Thin Films MOCVD制备Tl2Ba2Can-1CunO4+ 2n超导体和介电绝缘体薄膜
Pub Date : 1995-06-01 DOI: 10.1051/JPHYSCOL:1995546
B. Hinds, D. Studebaker, Jian‐Hong Chen, R. McNeely, B. Han, J. Schindler, T. Hogan, C. Kannewurf, T. Marks
The evolution of HTS device technologies will benefit from the development of MOCVD (Metal-organic Chemical Vapor Deposition) routes to high quality HTS films as well as to those of insulators with low dielectric loss and close HTS lattice matches. Reviewed here are research efforts at precursor design focusing on Ba sources. A novel low pressure TGA technique is used to compare volatilities of MOCVD precursors and to quantify the role of gas phase diffusion in film growth. To form high quality Tl 2 Ba 2 Ca n-1 Cu n O 4+2n (n = 2,3) films, BaCaCuO(F) films are first deposited by MOCVD using the liquid precursors Ba(hfa) 2 .mep, Ca(hfa) 2 .tet, and solid Cu(dpm) 2 (hfa = hexafluoroacetylacetonate, dpm = dipivaloylmethanate. mep = methylethylpentaglyme, tet = tetraglyme). The film growth process is shown to be mass transport-limited, and an interesting ligand exchange process is identified. The superconducting TBCCO phase is formed following an ex-situ anneal in the presence of Tl 2 O at temperatures from 820-900°C. Transport properties of TBCCO-2223 films include a T C as high as 115K. J C of 2x10 5 A/cm 2 (77K), and Rs of 0.35mΩ (5K, 10 GHz). The MOCVD growth of low loss, lattice-matched dielectric NdGaO 3 , PrGaO 3 , Sr 2 AlTaO 6 , and SrPrGaO 4 films is also discussed. High quality YBa 2 Cu 3 O 7-x films have been grown upon MOCVD-derived PrGaO 3 substrates.
高温超导器件技术的发展将受益于MOCVD(金属有机化学气相沉积)途径的发展,以获得高质量的高温超导薄膜,以及具有低介电损耗和接近高温超导晶格匹配的绝缘体。本文综述了以钡源为中心的前驱体设计的研究进展。采用一种新颖的低压热重分析技术来比较MOCVD前驱体的挥发性,并量化气相扩散在薄膜生长中的作用。为了制备高质量的Tl 2 Ba 2 Ca n-1 Cu n O 4+2n (n = 2,3)薄膜,首先采用MOCVD法制备了液态前驱体Ba(hfa) 2 .mep、Ca(hfa) 2 .tet和固态Cu(dpm) 2 (hfa =六氟乙酰丙酮酸,dpm =二戊基甲烷酸)。Mep =甲基乙基五烯酰胺,tet =四烯酰胺)。薄膜的生长过程受到质量输运的限制,并确定了一个有趣的配体交换过程。在tl2o存在下,在820 ~ 900℃的温度下进行非原位退火,形成超导TBCCO相。tbco -2223薄膜的输运性能包括高达115K的tc。jc为2 × 10 5a / cm2 (77K), Rs为0.35mΩ (5K, 10ghz)。本文还讨论了低损耗、晶格匹配介质NdGaO 3、PrGaO 3、Sr 2、AlTaO 6和SrPrGaO 4薄膜的MOCVD生长。在mocvd衍生的PrGaO 3衬底上生长了高质量的YBa 2 Cu 3 O 7-x薄膜。
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引用次数: 1
Thin Films of Zirconia-Phosphate Glasses Deposited by an Aerosol CVD Process 气溶胶气相沉积法制备磷酸锆玻璃薄膜
Pub Date : 1995-06-01 DOI: 10.1051/JPHYSCOL:19955121
J. Deschanvres, J. Vaca, J. Joubert
The polycrystalline state of the ZrO 2 films was an disadvantage for some specific protective coating applications. To resolve this fact we proposed to obtain an amorphous thin film by addition of P 2 O 5 , which will act as glass formator agent. With an aerosol CVD process by using zirconium acetylacetonate and triphenyl phosphate dissolved in a mixture of acetylacetone and benzyl alcohol, we achieved to deposit mixed P 2 O 5 -ZrO 2 films between 480°C and 600°C. The P 2 O 5 content varied from 0% up to 60%. By measuring systematically the composition of the film we have noticed the influence on the composition of the films, on the one hand of the hygrometric degree of the carrier gas and on the other hand of the temperature used for the dissolution of the organometallic precursors in the solvent. The highest the dissolution temperature was, the most the phosphorus content was. After an annealing at 500°C during one hour, the films exhibited by X-ray diffraction analysis an amorphous structure and a very good transparency. More over the evolution of the I.R. spectra between 1200 cm -1 and 900 cm -1 and around 400 cm -1 are discussed in function of the composition of the films.
zro2薄膜的多晶状态对某些特定的保护涂层应用是不利的。为了解决这一问题,我们提出通过添加p2o5作为玻璃形成剂来获得非晶薄膜。通过将乙酰丙酮锆和磷酸三苯酯溶解在乙酰丙酮和苯甲醇的混合物中,采用气溶胶气相沉积法,在480℃~ 600℃之间沉积了p2o -ZrO - 2混合薄膜。p2o5含量从0%到60%不等。通过系统地测量薄膜的组成,我们注意到载气的湿化程度和溶剂中溶解有机金属前驱体所用的温度对薄膜组成的影响。溶解温度越高,磷含量越高。经500℃退火1小时后,经x射线衍射分析,薄膜呈现出非晶态结构和良好的透明性。此外,本文还讨论了在1200 ~ 900 cm -1和400 cm -1之间的红外光谱随薄膜组成的变化。
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引用次数: 2
Preparation of Ultrafine CVD WC Powders Deposited from WCl6 Gas Mixtures WCl6混合气相沉积超细CVD WC粉末的制备
Pub Date : 1995-06-01 DOI: 10.1051/JPHYSCOL:19955119
Xing Tang, R. Haubner, B. Lux, B. Kieffer
Ultrafine WC powders were produced from WCl6-C3H8-H2 gaz mixtures in a conventional tubular hot-wall downstream CVD reactor. At reaction temperatures between 1100 and 1550°C powders containing W, W2C, WC and carbon were produced. The overall chemical compositions of the tungsten compounds as well as the free carbon contents depended strongly on the reaction temperature and the ratio of the reaction gases introduced. With increased reaction temperature and exposure time the amount of tungsten carbides (WC, W2C) in the deposits increased. At the selected conditions pure WC could be detected by X-ray diffraction. However, excess carbon was always present, while carbon particles could not be obsemed by SEM in the powder mixtures. This could be explained by thin carbon layers on the carbide particles. The WC powder particles were very fine but only particles or agglomerates smaller than 0.5 µm can be observed by SEM. A deposition mechanism based on reduction of the chlorides and their carburization to the carbides is discussed.
以WCl6-C3H8-H2气相混合物为原料,在常规管状热壁下游CVD反应器中制备超细WC粉末。在1100 ~ 1550℃的反应温度下,可制得含有W、W2C、WC和碳的粉末。钨化合物的总体化学组成和游离碳含量与反应温度和引入气体的比例有很大关系。随着反应温度的升高和暴露时间的延长,沉积物中碳化钨(WC、W2C)的含量增加。在选定的条件下,可以用x射线衍射检测到纯WC。然而,过量的碳总是存在,而碳颗粒在粉末混合物中无法通过扫描电镜观察到。这可以用碳化物颗粒上的薄碳层来解释。WC粉颗粒非常细,但扫描电镜只能观察到小于0.5µm的颗粒或团聚体。讨论了一种基于氯化物还原和渗碳的沉积机理。
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引用次数: 12
MOCVD of high quality YBa2Cu3O7−δ thin films using novel fluorinated and non-fluorinated precursors 采用新型氟化和非氟化前驱体制备高质量YBa2Cu3O7−δ薄膜
Pub Date : 1995-06-01 DOI: 10.1051/jphyscol:1995547
B. C. Richads, S. Cook, D. L. Pinch, G. W. Andrews
The first high quality, YBa 2 Cu 3 O 7-5 thin films have been produced by MOCVD using the novel fluorinated and non-fluorinated precursors, [Ba(TDFND) 2 .tetraglyme], [Cu(TDFND) 2 ] and [Y(TMHD) 3 .4- t BuPyNO] 2 and the traditional β-diketonate complexes [Y(TMHD) 3 ] 3 and [Cu(TMHD) 2 ]. The novel precursors are thermally stable and highly volatile. Their low melting points, 90 K and critical current density, J c > 10 6 Acm -2 at 77K. Fluorine content ∼100 ppm has been determined by SIMS.
利用新型氟化和非氟化前驱体[Ba(TDFND) 2 .四烯酰胺]、[Cu(TDFND) 2]和[Y(TMHD) 3 .4- t BuPyNO] 2以及传统的β-二酮酸配合物[Y(TMHD) 3] 3和[Cu(TMHD) 2],通过MOCVD法制备了第一个高质量的YBa 2 Cu 3 7-5薄膜。这种新型前体具有热稳定性和高挥发性。它们的熔点低,为90k,临界电流密度在77K时为jc > 10 6 Acm -2。氟含量~ 100 ppm已通过SIMS测定。
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引用次数: 0
Evolution of Magnetomechanical and Magnetic Properties of Siliconized Iron-Silicon Alloys by CVD Process Using SiCl4 用SiCl4 CVD工艺制备硅化铁硅合金的磁力学和磁性能演变
Pub Date : 1995-06-01 DOI: 10.1051/JPHYSCOL:19955123
S. Crottier-Combe, S. Audisio, J. Degauque, C. Béraud, Fausto Fiorillo, M. Baricco, J. Porteseil
Non-oriented and grain-oriented 6.5% Si-Fe laminations have been prepared by means of the dynamic Chemical Vapour Deposition technique, exploiting a chemical reaction at 1000°C between a flowing SiCl 4 + Ar mixture and an iron-silicon based substrate. The siliconizing process leads, from the first moments, to an epitaxial growth of Fe 3 Si, then to an underlayer solid solution by intermetallic diffusion. The optimum treatment has been chosen as 60 minutes at 1000°C, followed by 13 hour annealing in vacuum at the same temperature, which permits one to achieve the desired uniform concentration of Si around 6.5 wt %. NO and GO treated samples have been magnetically characterized in the frequency range 0.5 Hz - 1 kHz. A decrease between 15% and 50% of the energy loss has been observed in the CVD laminations.
通过动态化学气相沉积技术,利用流动的sicl4 + Ar混合物和铁硅基衬底在1000℃下发生化学反应,制备了无取向和晶粒取向的6.5% Si-Fe层状材料。硅化过程从最初的瞬间开始,导致Fe - 3si外延生长,然后通过金属间扩散形成底层固溶体。选择的最佳处理方法是在1000℃下60分钟,然后在相同温度下在真空中退火13小时,这样可以达到所需的均匀Si浓度,约为6.5 wt %。NO和GO处理的样品在0.5 Hz - 1 kHz的频率范围内进行了磁性表征。在CVD层合中观察到能量损失减少了15%至50%。
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引用次数: 1
Transmission Electron Microscopy Studies of (AIN-Si3N4) Codeposits Obtained by LPCVD LPCVD法制备(AIN-Si3N4)共沉积的透射电镜研究
Pub Date : 1995-06-01 DOI: 10.1051/JPHYSCOL:19955107
P. Marti, F. Henry, A. Mazel, B. Armas, J. Sévely
Several (Al,Si,N) compounds have been obtained by LPCVD in a vertical hot-wall reactor using aluminium trichloride, silicon tetrachloride and ammonia as source gases, with nitrogen as the carrier gas. In order to determine both their structure and local chemical composition, several deposits have been examined by analytical transmission electron microscopy combining electron diffraction (ED), high resolution electron microscopy (HREM) and electron energy loss spectroscopy (EELS). It has been confirmed that the chemical composition of the materials as well as the size of the nanocrystals observed in the deposits are strongly dependent on the temperature and the reactive gas flow. It has also been shown that for the range of temperature (1273 K-1373 K) used in this work these nanocrystals have the wurtzite structure of aluminium nitride.
以三氯化铝、四氯化硅和氨为源气体,以氮气为载气,在垂直热壁反应器中制备了几种(Al,Si,N)化合物。为了确定它们的结构和局部化学成分,用分析透射电子显微镜结合电子衍射(ED)、高分辨率电子显微镜(HREM)和电子能量损失谱(EELS)对一些沉积物进行了研究。已经证实,在沉积物中观察到的材料的化学成分以及纳米晶体的大小强烈依赖于温度和反应气体流量。研究还表明,在1273 K-1373 K温度范围内,这些纳米晶体具有氮化铝的纤锌矿结构。
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引用次数: 1
A Study of CVD of Gallium Nitride Films by In Situ Gas-Phase UV Spectroscopy 氮化镓薄膜CVD的原位气相紫外光谱研究
Pub Date : 1995-06-01 DOI: 10.1051/JPHYSCOL:1995520
S. Alexandrov, A. Kovalgin, D. Krasovitskiy
Direct in situ UV spectroscopic analysis of the gas phase was performed during chemical vapour deposition of gallium nitride films based on pyrolysis of GaCl 3 NH 3 complexes. The most probable mechanism of film formation is proposed on the basis of the experimental results obtained.
研究了基于gac3nh3配合物热解化学气相沉积氮化镓薄膜的气相直接原位紫外光谱分析。根据实验结果,提出了最可能的成膜机理。
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引用次数: 2
Comparison Between CVD and ALE Produced TiO2 Cathodes in Zn/(PEO)4ZnCl2/TiO2,SnO2 or ITO Galvanic Cells 在Zn/(PEO)4ZnCl2/TiO2、SnO2和ITO原电池中CVD和ALE制备TiO2阴极的比较
Pub Date : 1995-06-01 DOI: 10.1051/JPHYSCOL:19955134
A. Turkovic, A. Drašner, D. Šokčević, M. Ritala, T. Asikainen, M. Leskelä
The way of preparation of thin films of TiO 2 is extremely important regarding its application in electronic and optoelectronic devices. We have assembled Zn/(PEO) 4 ZnCl 2 /TiO 2 ,SnO 2 or ITO rechargeable galvanic cells using CVD (chemical vapour deposition) or ALE (atomic layer epitaxy) produced TiO 2 cathodes. The charge-discharge cycles were measured with a constant current in the range of 10 -6 to 10 -5 A for different cells. It was shown that CVD prepared TiO 2 cathode is increasing capacity of the cell by allowing higher constant currents to be applied to the cell. The complex impedance measurements of the electrolyte (PEO) 4 ZnCl 2 have been performed in the range of 1 Hz to 1 MHz and in the temperature range from 290 to 400 K by applying Zn or Sn electrodes.
二氧化钛薄膜的制备方法对其在电子和光电子器件中的应用至关重要。我们使用CVD(化学气相沉积)或ALE(原子层外延)生产的tio2阴极组装了Zn/(PEO) 4 ZnCl 2 / tio2,SnO 2或ITO可充电原电池。在10 -6 ~ 10 -5 a的恒流条件下,对不同的电池进行了充放电周期的测量。结果表明,CVD制备的二氧化钛阴极通过允许更高的恒定电流施加到电池上,从而提高了电池的容量。电解液(PEO) 4zncl2的复杂阻抗测量在1 Hz至1 MHz的范围内和290至400 K的温度范围内通过应用Zn或Sn电极进行。
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引用次数: 3
CVD Synthesis of HTSC Films Using Volatile Coordination Compounds 挥发性配位化合物CVD合成HTSC薄膜
Pub Date : 1995-06-01 DOI: 10.1051/JPHYSCOL:1995565
S. Volkov, V. Zub, O. N. Balakshina, E. Mazurenko
Thin HTSC films of YBa 2 Cu 3 O 7-x with high c-axis orientation have been grown using PE MOCVD technique and adducts of copper, yttrium and barium acetylacetonate with α,α'-dipyridyl as precursors. In-situ films were deposited in N 2 and O 2 gas reactant mixture at reduced substrate temperatures. HTSC films prepared on SrTiO 3 , ZrO 2 (Y) and MgO substrates have rather high electric characteristics (e.g. j c 10 4 - 10 5 A/cm 2 ). The problem of β-diketonate adducts using as precursors for plasma enhanced chemical vapor deposition of superconductive films was discussed.
采用PE MOCVD技术,以α,α′-二吡啶为前驱体,以乙酰丙酮酸铜、钇和钡为加合物,制备了具有高c轴取向的yba2cu3o7 -x HTSC薄膜。在降低衬底温度的条件下,在n2和o2气体反应物混合物中沉积原位膜。在SrTiO 3, ZrO 2 (Y)和MgO衬底上制备的HTSC薄膜具有相当高的电特性(例如jc10 4 - 10 5 A/ cm2)。讨论了β-二酮酸加合物作为等离子体增强化学气相沉积超导薄膜前驱体的问题。
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引用次数: 0
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Le Journal De Physique Colloques
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