Measurements of Thermal Conductivity and Thermal Diffusivity of CVD Diamond

The thermal conductivity of natural, gem-quality diamond, which can be as high as 2500 Wm^–1 K^–1 at 25°C, is the highest of any known material. Synthetic diamond grown by chemical vapor deposition (CVD) of films up to 1 mm thick exhibits generally lower values of but under optimal growth conditions it can rival gem-quality diamond with values up to 2200 Wm^–1 K^–1. However, it is polycrystalline and exhibits a columnar microstructure. Measurements on free-standing CVD diamond, with a thickness in the range 25–400 m, reveal a strong gradient in thermal conductivity as a function of position z from the substrate surface as well as a pronounced anisotropy with respect to z. The temperature dependence of in the range 4 to 400 K has been analyzed to determine the types and numbers of phonon scattering centers as a function of z. The defect structure, and therefore the thermal conductivity, are both correlated with the microstructure. Because of the high conductivity of diamond, these samples are thermally thin. For example, laser flash data for a 25-m-thick diamond sample is expected to be virtually the same as laser flash data for a 1-m-thick fused silica sample. Several of the techniques described here for diamond are therefore applicable to much thinner samples of more ordinary material.     

Thermal diffusivity measurement of CVD diamond film using a step heating technique

A step heating method for the measurement of the thermal diffusivity of diamond thin film is described. The step heating method is a transient heat flow method. Transient temperature profiles are generated in a strip-shaped sample by heating one end of the sample while the other end is clamped to a heat sink. Three thermocouples are used along the heat path. The results are compared with the literature values over the temperature range from –190 to 50°C.     

Thermal Diffusivity of Diamond Wafers Deposited with Multicathode dc Plasma-Assisted CVD

A thermal diffusivity map for diamond wafers of 10-cm diameter was obtained using a converging thermal wave technique in a nondestructive and noncontact manner. Diamond wafers were deposited by seven-cathode dc plasma-assisted chemical vapor deposition with different CH₄concentrations in pure hydrogen and applied powers of the plasma. Six cathodes were located at the apexes of a hexagon with an arm distance of 4.3 cm about a central cathode. The wafer deposited at a low-power plasma (13.47 kW) and a low concentration of CH₄(6%, by volume) shows three circular zones on the thermal diffusivity map. The thermal diffusivity shows the lowest value at the center. It increases to about 10% in a radius of 2 to 3 cm and then decreases with further increases in the radius. The optical photograph and the Raman lines of the wafer show patterns similar to those of the thermal diffusivity. These are affected by the locations of the cathodes in the deposition chamber when the plasma power is low. Diamond wafers deposited at a high-power plasma (20.58 kW) with high concentrations of methane (10%, by volume) show higher values of thermal diffusivity and better uniformity than wafers deposited at a low power and low methane concentration. A fine crack can be located on a wafer with the converging thermal wave technique.     

CVD金刚石膜的场发射机制

利用热灯丝化学气相沉积方法在光滑的钼上沉积了金刚石膜,用扫描电子显微镜和Raman谱对金刚石膜进行了分析。结果表明金刚石膜是由许多金刚石晶粒组成,晶粒间界主要是石墨相,并且在膜内有许多缺陷。金刚石膜的场发射结果表明高浓度CH4形成的金刚石膜场发射阈位电场较低浓度CH4形成的金刚石为低。这意味着杂质（如石墨）和缺陷（悬挂键）极大地影响了膜的场发射性能。根据以上结果,提出了一种CVD金刚石膜的场发射机制即膜内的缺陷增强膜内的电场,石墨增大电子的隧穿系数以增强CVD金刚石膜的场发射。     

Correction of Edge Effect in AC Calorimetric Method for Measuring Thermal Diffusivity of CVD Diamond Films1

In the thermal diffusivity measurement of a CVD diamond film using an ac calorimetric method, the reflection of an ac temperature wave at the edge of the film sample should be considered due to the limited length of the sample and its high thermal diffusivity, i.e., the edge effect. In this case, the measured thermal diffusivity is given as a function of frequency. The relation between the measured thermal diffusivity and the frequency is represented as an analytical expression. The real thermal diffusivity is obtained by correcting the edge effect by two means. One is an iterative method using the directly measured edge length of the sample to fit the analytical expression. The other is a parameter estimation method by which a simplex method is used to estimate the edge length and the real thermal diffusivity. Thermal diffusivities of two diamond films were measured, and data were analyzed using the above methods. The result shows that the parameter estimation method is relatively accurate and convenient in processing test data.     

大面积高质量金刚石自支撑膜热导率的影响因素研究

通过Raman、XRD、SEM分析方法分别对大面积高质量金刚石自支撑膜的质量、晶体结构、晶粒尺寸进行研究,分析它们对金刚石自支撑膜热导率的影响.研究结果表明,金刚石自支撑膜的质量对热导率的影响较大,质量越好,热导率越接近于天然金刚石的热导率;并且金刚石自支撑膜中晶体[220]取向度越高,热导率越高.形核面晶粒尺寸越大,晶粒间的晶界就减少,有利于提高金刚石自支撑膜的热导率.     

Thermal Diffusivity by Modified ac Calorimetry Using a Modulated Laser Beam Energy Source

Modified ac calorimetry, a variation of the Angstrom method, has been shown to be a precise tool for measuring the in-plane thermal diffusivity of thin films (thickness less than 300 m) of a wide variety of materials and layered composites. The property is determined from an analysis of the decay curve of the ac temperature waves generated by irradiation of a specimen using uniform chopped light (at frequencies from 1 to 20 Hz) from a halogen lamp source. To address certain limiting factors, especially to improve the signal-to-noise ratio and to eliminate heat losses, an improved form of measurement instrument has been developed. It is based on the use of a modulated laser beam heating to provide a higher intensity energy source plus a special optical system to ensure that one-dimensional ac temperature wave propagation is obtained. Measurements can now be made using frequencies in the range of 0.01 to 10 Hz, i.e., 10 times lower than in the traditional method. The performance of the improved measurement instrument will be illustrated by results on various materials of known thermal properties such as nickel and stainless steel, proposed reference materials such as a glassy carbon and alumina, plus a comparison of results obtained on CVD diamond films used in an international round-robin series with those obtained by the traditional technique.     

熔融铈快速抛光CVD金刚石厚膜及表面分析

利用熔融稀土铈(Ce)对CVD金刚石厚膜进行了抛光研究.详细讨论了工艺参数对抛光速率和表面粗糙度Ra的影响,获得了最佳抛光工艺.通过对抛光后金刚石膜表面的拉曼光谱(Raman)、俄歇能谱(AES)、扫描电镜(SEM)以及能谱(EDS)的分析,探讨了抛光机理.结果表明:该方法有很高的抛光速率,可达每小时数百微米.抛光后金刚石膜的Ra从10.845μm降低至0.6553μm.抛光的热处理工艺不但没有破坏金刚石表面的原始结构,而且由于铈对石墨的优先刻蚀,抛光后金刚石膜表面的石墨含量还大大减少.     

Effects of enhanced nucleation on the growth and thermal performance of diamond films deposited on BeO by hot filament CVD technique

A method of controlling the feeding concentration of methane was applied in a hot-filament chemical vapor deposition (HFCVD) in order to improve the nucleation of diamond on the beryllium oxide substrates. The nucleation density and the morphologies of diamond were investigated by scanning electron microscopy (SEM) and atomic force microscopy (AFM) while the thermal conductivities of substrates and the composites were detected by laser-diathermometer. The results show that the diamond thin film is in larger grain size with lower roughness when CH₄ and H₂ enter the chamber, respectively, rather than as a mixture, and the composites’ conductivity soared by 21%–31% compared with BeO substrates. At the conditions of separated gas entry, several projects with changes of the CH₄ flux during depositing were designed to discuss the influence of CH₄ concentration on diamond nucleation. The uniform and compact diamond thin films were acquired when the ratio of CH₄:H₂ at nucleation stage was in the range of 4%–8%.     

化学气相沉积金刚石薄膜生长的原位反射率测量

报道了化学气相沉积金刚石薄膜生长的原位反射率测量,提出了监控金刚石薄膜生长的激光反射多光束干涉的数学模型。通过原位反射率的测量,精确监控了金刚石薄膜的生长厚度,成功地制备了红外增透增,这种方法的测量装置简单、紧凑而且可靠。     

Temperature-Dependent Thermal Conductivity of Undoped Polycrystalline Silicon Layers

Polycrystalline silicon is used in microelectronic and microelectromechanical devices for which thermal design is important. This work measures the in-plane thermal conductivities of free-standing undoped polycrystalline layers between 20 and 300 K. The layers have a thickness of 1 m, and the measurements are performed using steady-state Joule heating and electrical-resistance thermometry in patterned aluminum microbridges. The layer thermal conductivities are found to depend strongly on the details of the deposition process through the grain size distribution, which is investigated using atomic force microscopy and transmission electron microscopy. The room-temperature thermal conductivity of as-grown polycrystalline silicon is found to be 13.8 W·m^-1·K^-1and that of amorphous recrystallized polycrystalline silicon is 22 W·m^-1·K^-1, which is almost an order of magnitude less than that of single-crystal silicon. The maximum thermal conductivities of both samples occur at higher temperatures than in pure single-crystalline silicon layers of the same thickness. The data are interpreted using the approximate solution to the Boltzmann transport equation in the relaxation time approximation together with Matthiessen's rule. These measurements contribute to the understanding of the relative importance of phonon scattering on grain and layer boundaries in polysilicon films and provide data relevant for the design of micromachined structures.     

n-Type CVD diamond: Epitaxy and doping

Diamond is a semiconductor with superlative properties in terms of operating temperature, breakdown voltage and thermal dissipation for high power electronic applications. The p-type doping is currently controlled but it is not the case for the n-type doping. In spite of the low solubility of substitutional donors bigger than carbon, n-type material can be achieved via impurity doping during the growth of diamond with phosphorus dopant (E_c = 0.6 eV). Theoretical studies also predict arsenic as a shallower dopant (E_c = 0.4 eV). This paper outlines the n-type doping issues with phosphorus and explores the arsenic doping.     

金刚石薄膜热导率的研究现状

分析了金刚石薄膜热导率的声子导热机理,从金刚石薄膜晶体结构的角度总结了影响热导率的因素,例如晶界、晶内杂质、缺陷、晶粒尺寸、晶粒取向、同位素;从金刚石薄膜合成工艺角度探讨了影响金刚石薄膜热导率的因素,例如基底材料及预处理、合成温度、气源及添加气体(氧气、氮气)、工作压强、功率等.     

Thermal conductivity of Cu-4.5 Ti alloy

The thermal conductivity (TC) of peak aged Cu-4.5 wt% Ti alloy was measured at different temperatures and studied its variation with temperature. It was found that TC increased with increasing temperature. Phonon and electronic components of thermal conductivity were computed from the results. The alloy exhibits an electronic thermal conductivity of 46.45 W/m.K at room temperature. The phonon thermal conductivity decreased with increasing temperature from 17.6 at 0 K to 1.75 W/m.K at 298 K, which agrees with literature that the phonon component of thermal conductivity is insignificant at room temperature.     

Thermal diffusivity and conductivity in low-conducting materials: A new technique

A comparative method is presented, suitable to measure both thermal diffusivity and conductivity of low-conducting solids. The repeatibility of the measurements of thermal conductivity is 3%, whereas for diffusivity is 6%. Data for some low-conducting materials are given, consistent with those reported in the literature.     

晶粒尺寸对CVD金刚石膜电学特性的影响

通过改变生长参数,采用热丝化学气相沉积(HFCVD)法制备了从10μm到90nm四种晶粒尺寸的金刚石膜,并制作了三明治结构的光电导探测器.采用原子力显微镜和拉曼光谱仪研究了薄膜的结构和表面形貌:表面粗糙度从423nm变化到15nm;晶粒越大,金刚石膜的质量越好.I-V特性测试结果表明随着晶粒尺寸的减小,金刚石膜的电阻率从1011Ω·cm减小到106Ω·cm.在5.9 keV的55Fe X射线辐照下,随着晶粒尺寸的减小,探测器的信噪比(SNR)呈减小趋势.     

器件级同质外延CVD金刚石膜上的具有高击穿电压的铝肖特基二极管

用微波等离子体化学气相沉积方法合成高品质同质外延金刚石膜,并且用扫描电镜和阴极荧光分析法评价。为了得到高薄膜生长速率,把甲烷浓度设定在4%。薄膜上的生长丘的数量和大小依赖于生长条件。在本工作的样品中,未发现任何非外延晶粒。室温下的阴极荧光分光结果表明这种金刚石薄膜具有与自由励起子相关的谱峰。氢终端的膜表面制作的铝电极显示了P型整流特性。击穿电压高于380V。实验结果表明,阴极荧光分析法观测到的缺陷和电性能密切相关,并且可以在有室温边发射的金刚石表面上制作具有高击穿电压的整流电极。     

金刚石薄膜生长速度研究

在电子辅助热丝CVD中,研究刀具预处理对金刚石薄膜生长速度的影响。在保持生长条件不变的前提下,经酸腐蚀处理的刀具的侧、背面镀铜能使金刚石薄膜的生长速度从没有镀铜时的4μm／h增加到镀铜后的10．6μm／h。镀铜处理提高了刀具的电导率,使得热丝发射的电子在偏压电场的作用下,在刀具表面附近聚集,加速氢气和丙酮的裂解,从而提高金刚石薄膜生长速度。SEM和Raman测试结果表明,高速生长的金刚石薄膜仍然具有很高质量。     

Thermal conductivity and diffusivity measurements at cryogenic temperatures by double specimen technique

A double specimen technique is used in measuring the thermal conductivity and diffusivity of low thermal conductivity materials. In this technique good thermal contact is maintained between the heat source and sink and two geometrically similar specimens. A thin-copper heater plate is compressed between the two specimens and the temperature difference is measured between the heat source and the temperature controlled heat sink. Thermal conductivity is determined at steady state conditions by the differential method while the diffusivity is determined from transient measurements combined with an analytical solution to the one dimensional solution of the diffusion equation.     

Measurements of Thermal Diffusivity for Thin Slabs by a Converging Thermal Wave Technique

The measurement of thermal diffusivity for thin slabs by a converging thermal wave technique has been studied. Temperature variation at the center of the heat source ring that is produced by a pulsed high-power laser is detected by an infrared detector. A computer program based on the finite difference method is developed to analyze the thermal diffusivity of the slabs. Materials of both high thermal diffusivity (CVD diamond wafer) and low thermal diffusivity (stainless-steel foil) have been used for the measurements. The measurements have been performed by varying the size and the thickness of specimen. The converging thermal wave technique has proved to be a good method to measure the thermal diffusivity of a CVD diamond without breaking the wafer into small specimens. The technique can be applied for a small slab if the diameter of the slab is two times larger than that of the heat source ring. The sensitivity of thickness in measuring the thermal diffusivity is low for ordinary CVD diamond. The use of the converging thermal wave technique for nonhomogeneous, nonuniform, and anisotropic materials has been accomplished by applying the finite difference method.