Determination of the thermal conductivity of polycrystalline diamond films by means of the photoacoustic effect

A new method of determining the heat-conducting properties of diamond films is proposed, based on the photoacoustic effect. This method is used to study diamond polycrystalline films grown on silicon by chemical vapor deposition in a microwave discharge plasma. The thermal conductivity obtained was approximately half that for single-crystal diamond. Zh. Tekh. Fiz. 69, 97–101 (April 1999)     

Investigation of the thermal conductivity of diamond film on aluminum nitride ceramic

Diamond films were successfully synthesized on aluminum nitride(AlN) ceramic substrates by hot-filament chemical vapor deposition (HFCVD) method. The thermal conductivity of the diamond film/aluminum nitride ceramic (DF/AlN) composites was studied by photothermal deflection (PTD) technique. It has reached 2.04 W/cm K, 73% greater than that of AlN ceramic. Compared with the measurement of scanning electron microscopy (SEM) and Raman spectroscopy, the influence of diamond films on the thermal conductivity of the composites was pointed out. The adhesion and the stresses were also studied. The unusual stability and very good adhesion of the diamond film on AlN ceramic substrate obtained is attributed to the formation of aluminum carbide. Received: 24 March 1998 / Accepted: 8 March 1999 / Published online: 5 May 1999     

Particle size effect on thermal conductivity of AlN films with embedded diamond particles

Fabricating composite thin films is an effective and economic solution to improve the thermal performance of the films. The diamond particles of different sizes were successfully embedded in AlN thin films by a chemical solution approach, which was confirmed by scanning electron microscope, x-ray diffraction analysis and x-ray photoelectron spectroscopy. The thermal properties of the films embedded with different diamond particles were studied by using a 3-omega method, which was observed to be strongly dependent on the particle size. A 19 % enhancement in thermal conductivity can be achieved by embedding diamond particles of 1-μm radius in AlN thin films. However, the thermal conductivity decreases after embedding with 10-nm radius diamond particles. The results are discussed with high volume model, which confirms that the interface thermal resistance between the embedded materials and the films plays an important role in determining the thermal conductivity of the as-grown carbon material embedded AlN films.     

Influence of structural characteristics on the thermal conductivity of polycrystalline diamond films

By analyzing the signal formed by the photoacoustic effect as a function of the light modulation frequency, it is shown that this effect may be used to determine the thermal conductivity of diamond materials. The method is checked experimentally for two types of polycrystalline diamond films grown by chemical vapor deposition with the gaseous medium activated by a dc discharge and a microwave discharge. The data obtained on the thermal conductivity of the films are discussed with reference to the results of an investigation of the optical absorption, Raman light scattering, and cathodoluminescence of similar films. It is shown that the thermal conductivity of polycrystalline diamond films depends on the structural characteristics, which are determined by the deposition conditions. Fiz. Tverd. Tela (St. Petersburg) 40, 1221–1225 (July 1998)     

吸收辐射复合金刚石膜的制备及光学研究

采用微波等离子体化学气相沉积（MW-PCVD）和直流热阴极辉光放电等离子体化学气相沉积（DC-PCVD）两种方法相结合,制备出一种吸收辐射的复合金刚石膜,它对宽光谱范围的光辐射具有99%—99.2%的吸收率,同时具有较低的反射率和透过率.随着黑色吸收辐射金刚石层厚度的增加,复合金刚石膜的热导率将小幅度降低,但黑色金刚石膜层厚度小于15 μm时,复合金刚石膜的热导率都在16 W·cm^-1·K^-1以上,这满足吸收辐射复合金刚石膜的高导热需求.用热阴极DC-PCVD方 关键词： 吸收辐射 光学材料 金刚石 热导率     

高导热金刚石薄膜的研究

分析了影响金刚石膜热导率的主要因素，指出声子的散射是造成金刚石膜热导率降低的主要原因．采用光热偏转法实现了金刚石薄膜热导率的测试，测量误差小于5%，从减少杂质和晶界对导热声子的散射入手，研究了在不同的制备方法下碳源气体和金刚石膜内晶粒取向对其热导率的影响．结果表明在低碳源气体浓度下采用微波等离子体化学汽相沉积方法制备的具有较高程度（400）晶粒取向的金刚石薄膜具有高的热导率性质．优化的工艺条件制备出热导率为15.2W/（K·cm）左右的金刚石膜． 关键词：     

Effect of nanostructured AlN coatings on the oxidation-resistant properties of optical diamond films

Diamond film is an ultra-durable optical material with high thermal conductivity and good transmission in near-infrared and far-IR (8-14 μm) wavebands. CVD diamond is subjected to oxidation at temperature higher than 780 °C bared in air for 3 min, while it can be protected from oxidation for extended exposure in air at temperature up to 900 °C by a coating of aluminum nitride. Highly oriented AlN coatings were prepared for infrared windows on diamond films by reactive sputtering method and the average surface roughness (R_a) of the coatings was about 10 nm. The deposited films were characterized by X-ray diffraction (XRD) and atom force microscope (AFM). XRD confirmed the preferential orientation nature and AFM showed nanostructures. Optical properties of diamond films coated AlN thin film was investigated using infrared spectrum (IR) compared with that for as-grown diamond films.     

Thermal conductive performance of deposited amorphous carbon materials by molecular dynamics simulation

A series of diamond-like carbon (DLC) films with different microstructure were prepared by depositing carbon atoms on diamond surface with incident energy ranging from 1 to 100 eV. The thermal conductivity of the deposited films and the Kapitza resistance between the film and the diamond substrate were investigated. Results show that the average density, the average fraction of sp³ bonding and the thermal conductivity of the DLC films increase first, reaching a maximum around 20–40 eV before decreasing, while the Kapitza resistance decreases gradually with increased deposition energy. The analysis suggests that the thermal resistance of the interface layer is in the order of 10^?10 m²K/W, which is not ignorable when measuring the thermal conductivity of the deposited film especially when the thickness of the DLC film is not large enough. The fraction of sp³ bonding in the DLC film decreases gradually normal to the diamond surface. However, the thermal conductivity of the film in normal direction is not affected obviously by this kind of structural variation but depends linearly on the average fraction of sp³ bonding in the entire film. The dependence of the thermal conductivity on the fraction of sp³ bonding was analysed by the phonon theory.     

Off-axis Thermal Properties of Carbon Nanotube Films

Theoretical calculations have predicted that individual Single-Walled Carbon Nanotubes (SWNT) have extremely high thermal conductivity (around 6.6 × 10⁴ W/m-K). The feasibility of constructing practical devices using the above mentioned properties, is critically dependent on the ability to synthesize high-thermal-conducting films. Highly conducting films would be of great use as heat sinks for the next generation of integrated chips. Excessive heating is currently a very serious problem in the endeavor for achieving faster and smaller chips. Since it is still not possible to perfectly align SWNT in the macroscopic scale, the thermal properties of the nano-films are therefore expected to have a statistical effect and thus lower than the intrinsic thermal conductivity of a single nanotube. Also the thermal conductivity perpendicular to the tube direction is more significant from a practical point of view. Multi-Walled Carbon Nanotubes (MWNT) were synthesized by Chemical Vapor Deposition (CVD) technique and subsequently characterized. The thin MWNT films were deposited by a solution casting technique over a metallic substrate. The off-axis thermal properties of these nano-films were studied by AC-calorimetry studies. In this method, the sample is heated by an AC source and the measurement of the relaxation rate is used to determine the thermal properties. This technique is well established for studying the thermal properties of complex fluids. Our results are contrasted with other thermal conductivity measurements intrinsic and bulk carbon nanotube samples. We have also measured off-axis thermal properties of nano-films synthesized from more crystalline SWNT samples and have compared this result with that of the MWNT-film. A model to explain the thermal conduction for our system is proposed. George Muench: Presently at the Department of Physics, University of New Haven, West Haven, CT-06516, USA     

Comparative study of textured diamond films by thermal conductivity measurements

Superior thermal conductivity, high resistance, high breakdown voltage and wide band gap make diamond an attractive material for a variety of applications in electronics. One of its most appealing applications is as a buried dielectric in silicon-on-diamond (SOD) technology. This paper presents thermal conductivity measurements conducted on a series of diamond films (grown by the microwave plasma chemical vapor deposition technique) as a function of the sample morphology and thickness, for eventual incorporation in the SOD structures. Results show that there is a significant difference in the measured thermal conductivity between samples with fiber texture and samples with sheet texture. Also, measurements performed on a 160-μm-thick diamond sample before and after reactive ion etching of approximately 10 μm of the nucleation layer show no significant change in the measured value of the thermal conductivity. PACS 81.05.Uw; 65.40.-b; 61.72.-y     

微尺度薄膜热导率测试技术

随着器件尺寸进入到微／纳米尺度，其热物性与体材料相比有了很大差别。在器件热性能和可靠性研究过程中，对热导率的测量成为了关键技术之一。本文概述了SiO2、SiNx、金刚石等薄膜在微小型器件中的用途及其热导率测试技术的发展，并进一步总结了用于薄膜热导率测量的常用方法。     

SiNx薄膜热物性参数实验测量与分析研究

采用一种新的实验测量方案，将金属加热单元与温度探测单元合二为一，间接获得了在半导体和微电子学MEMS领域内有重要用途的SiN_x薄膜的导热系数、发射率、比热容和热扩散系数，并对实验结果进行了不确定度分析，为微电子电路设计和掩模成型工艺等提供了可靠的热物性数据. 实验结果表明，薄膜的导热系数、发射率、热扩散系数远比相应体材质低，而且还与温度、厚度有关，尺寸效应显著，而比热容则与体材质相差不大. 关键词： 微尺度传热 热物性参数 x薄膜')" href="#">SiN_x薄膜 测量技术     

Photoacoustic spectroscopy of diamond powders and polycrystalline films

Photoacoustic spectroscopy is used to study optical absorption in diamond powders and polycrystalline films. The photoacoustic spectra of diamond powders with crystallite sizes in the range from ∼100 μm to 4 nm and diamond films grown by chemical vapor deposition (CVD) had a number of general characteristic features corresponding to the fundamental absorption edge for light with photon energies exceeding the width of the diamond band gap (∼5.4 eV) and to absorption in the visible and infrared by crystal-structure defects and the presence of non-diamond carbon. For samples of thin (∼10 μm) diamond films on silicon, the photoacoustic spectra revealed peculiarities associated with absorption in the silicon substrate of light transmitted by the diamond film. The shape of the spectral dependence of the amplitude of the photoacoustic signal in the ultraviolet indicates considerable scattering of light specularly reflected from the randomly distributed faces of the diamond crystallites both in the polycrystalline films and in the powders. The dependence of the shape of the photoacoustic spectra on the light modulation frequency allows one to estimate the thermal conductivity of the diamond films, which turns out to be significantly lower than the thermal conductivity of single-crystal diamond. Fiz. Tverd. Tela (St. Petersburg) 39, 1787–1791 (October 1997)     

Ultra‐thin nanocrystalline diamond films (<100 nm) with high electrical resistivity

Thick diamond films are known to exhibit remarkably high electrical resistivity and thermal conductivity. However, on thin films, difficulties are often observed to achieve such performances. In this study, the synthesis of ultra‐thin diamond films was optimized towards the possibility to maintain high dielectric performances on layers compatible with today requirements for Silicon‐On‐Diamond technology, and namely aiming at films with thicknesses equal or below 150 nm. The nucleation of diamond nanocrystals is crucial to obtain films with thickness lower than 100 nm. A Bias Enhanced Nucleation step (BEN) was improved to achieve nucleation densities above 10¹¹ cm^–2 although the process was also tuned to limit the size of the nanocrystals during this step. The control of the carbonization of the silicon substrate is also essential to reach such a density with a high reproducibility. The BEN is followed by a growth step with optimized conditions. The films were characterized by SEM and Spectroscopic Ellipsometry. Electrical conductivity measurements were conducted on thin diamond films and values obtained on layers below 100 nm were as high as 5 × 10¹³ Ω cm; a value significantly higher than the state of the art for such thin films. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Thermal conductivity of hcp iron at high pressure and temperature

Results of steady-state heat transfer experiments on iron in laser-heated diamond anvil cell, combined with numerical simulation using finite-element method are reported. Thermal boundary conditions, dimensions of sample assemblage, heating-laser beam characteristics and relevant optical properties have been well defined in the course of experiments. The thermal conductivity of the polycrystalline hexagonal-iron foil has been determined up to pressure 70 GPa and temperature 2000 K. At these conditions, the conductivity value of 32±7 W/m K was found. Sources of errors arising from uncertainties in input parameters and applied experimental procedures are discussed. Considering results of earlier preferred-orientation studies in diamond anvil cell, an averaging effect of polycrystalline texture on the intrinsic anisotropy is assumed. The obtained conductivity is interpreted as an effective value, falling in between the upper and lower bounds on the average conductivity of a random aggregate of uniaxial crystals.     

退火温度对硼掺杂纳米金刚石薄膜微结构和p型导电性能的影响

采用热丝化学气相沉积法制备硼掺杂纳米金刚石 (BDND) 薄膜, 并对薄膜进行真空退火处理, 系统研究退火温度对BDND薄膜微结构和电学性能的影响. Hall效应测试结果表明掺B浓度为5000 ppm (NHB) 的样品的电阻率较掺B浓度为500 ppm (NLB) 的样品的低, 载流子浓度高, Hall迁移率下降. 1000 ℃退火后, NLB和NHB 样品的迁移率分别为53.3和39.3 cm²·V^-1·s^-1, 薄膜的迁移率较未退火样品提高, 电阻率降低. 高分辨透射电镜、紫外和可见光拉曼光谱测试结果表明, NLB样品的金刚石相含量较NHB样品高, 高的硼掺杂浓度使薄膜中的金刚石晶粒产生较大的晶格畸变. 经1000 ℃退火后, NLB和NHB薄膜中纳米金刚石相含量较未退火时增大, 说明薄膜中部分非晶碳转变为金刚石相, 为晶界上B扩散到纳米金刚石晶粒中提供了机会, 使得纳米金刚石晶粒中B浓度提高, 增强纳米金刚石晶粒的导电能力, 提高薄膜电学性能. 1000 ℃退火能够恢复纳米金刚石晶粒的晶格完整性, 减小由掺杂引起的内应力, 从而提高薄膜的电学性能. 可见光Raman光谱测试结果表明, 1000℃退火后, Raman谱图中反式聚乙炔 (TPA) 的1140 cm^-1峰消失, 此时薄膜电学性能较好, 说明TPA减少有利于提高薄膜的电学性能. 退火后金刚石相含量的增大、金刚石晶粒的完整性提高及TPA含量的大量减少有利于提高薄膜的电学性能. 关键词： 硼掺杂纳米金刚石薄膜 退火 微结构 电学性能     

Ionic conductivity, thermal stability and FT-IR studies on plasticized PVC / PMMA blend polymer electrolytes complexed with LiAsF6 and LiPF6

The lithium salt (x) (x=LiAsF₆, LiPF₆) was complexed with a blend of poly(vinyl chloride) (PVC) / poly(methyl methacrylate)(PMMA) and plasticized with a combination of ethylene carbonate(EC) and propylene carbonate(PC). The electrolyte films were prepared using doctor blade method and subjected to ionic conductivity measurements at nine different temperatures viz.,-30, -15, 0, 15, 30, 40, 50, 60 and 70 °C. The films were also subjected to TG - DTA and FT-IR analysis. The effect of salt on ionic conductivity is discussed. A 75:25 PMMA/PVC blend at 60 % plasticizer content has been found to possess optimal properties in terms of ionic conductivity, thermal and electrochemical stability.     

Classical and photopyroelectric studies of optical and thermophysical properties of starch sheets: dependence on water content and temperature

The optical and thermophysical parameters of starch films (obtained by extrusion) were determined in order to obtain input data for photothermal studies of water migration in such films. The optical spectra, sorption isotherm, and volume change were measured for samples equilibrated at different levels of relative humidities. The photopyroelectric method was used to measure thermal parameters as a function of water content and temperature. The thermal conductivity, thermal effusivity, and volume specific heat all increase with water content while the thermal diffusivity remains almost constant. The temperature behaviour of the thermal parameters in the -15+70 °C temperature range was measured for samples with different water contents. No phase transition was observed at 0 °C, which proves either that water in the starch matrix is not in a free form, or the fact that water dissolved other particles shifting the melting point to a lower temperature. Received: 1 June 1999 / Final version: 13 March 2000 / Published online: 7 June 2000     

Electronic structures of phosphorus-doped diamond films and impacts of their vacancies

In order to better understand the bonding mechanisms of the phosphorus-doped diamond films and the influences of the phosphorus-doped concentration on the diamond lattice integrity and conductivity,we calculate the electronic structures of the phosphorus-doped diamond with different phosphorus concentrations and the density of states in the phosphorus--doped diamond films with a vacant lattice site by the first principle method.The calculation results show the phosphorus atom only affects the bonds of a few atoms in its vicinity,and the conductivity increases as the doped concentration increases.Also in the diamond lattice with a total number of 64 atoms and introducing a vacancy into the non-nearest neighbor lattice site of a phosphorus atom,we have found that both the injuries of the phosphorus-doped diamond films and the N-type electron conductivity of diamond films could be improved.     

Thermal conductivity of polycrystalline CVD diamond: Experiment and theory

The temperature dependences of thermal conductivity κ of polycrystalline CVD diamond are measured in the temperature range from 5 to 410 K. The diamond sample is annealed at temperatures sequentially increasing from 1550 to 1690°C to modify the properties of the intercrystallite contacts in it. As a result of annealing, the thermal conductivity decreases strongly at temperatures below 45 K, and its temperature dependence changes from approximately quadratic to cubic. At T > 45 K, the thermal conductivity remains almost unchanged upon annealing at temperatures up to 1650°C and decreases substantially at higher annealing temperatures. The experimental data are analyzed in terms of the Callaway theory of thermal conductivity [9], which takes into account the specific role of normal phonon-phonon scattering processes. The thermal conductivity is calculated with allowance for three-phonon scattering processes, the diffuse scattering by sample boundaries, the scattering by point and extended defects, the specular scattering by crystallite boundaries, and the scattering by intercrystallite contacts. A model that reproduces the main specific features of the thermal conductivity of CVD diamond is proposed. The phonon scattering by intercrystallite contacts plays a key role in this model.