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This chapter describes the nature of clean and contaminated diamond surfaces, Chemical-vapor-deposited (CVD) diamond film deposition technology, analytical techniques and the results of research on CVD diamond films, and the general properties of CVD diamond films. Further, it describes the friction and wear properties of CVD diamond films in the atmosphere, in a controlled nitrogen environment, and in an ultra-high-vacuum environment.
Semiconducting diamond films have the potential for use as a material in which to build active electronic devices capable of operating at high temperatures or in high radiation environments. Ultimately, it is preferable to use low-defect-density single crystal diamond for device fabrication. We have previously investigated polycrystalline diamond films with transmission electron microscopy (TEM) and scanning electron microscopy (SEM), and homoepitaxial films with SEM-based techniques. This contribution describes some of our most recent observations of the microstructure of natural diamond single crystals and homoepitaxial diamond thin films using TEM.
A diamond turning process has made possible a significant advance in the art of whispering-gallery-mode (WGM) optical resonators. By use of this process, it is possible to fashion crystalline materials into WGM resonators that have ultrahigh resonance quality factors (high Q values), are compact (ranging in size from millimeters down to tens of microns), and support single electromagnetic modes. This development combines and extends the developments reported in "Few- Mode Whispering-Gallery-Mode Resonators" (NPO-41256), NASA Tech Briefs, Vol. 30, No. 1 (January 2006), page 16a and "Fabrication of Submillimeter Axisymmetric Optical Components" (NPO-42056), NASA Tech Briefs, Vol. 31, No. 5 (May 2007), page 10a. To recapitulate from the first cited prior article: A WGM resonator of this special type consists of a rod, made of a suitable transparent material, from which protrudes a thin circumferential belt of the same material. The belt is integral with the rest of the rod and acts as a circumferential waveguide. If the depth and width of the belt are made appropriately small, then the belt acts as though it were the core of a single-mode optical fiber: the belt and the rod material adjacent to it support a single, circumferentially propagating mode or family of modes. To recapitulate from the second cited prior article: A major step in the fabrication of a WGM resonator of this special type is diamond turning or computer numerically controlled machining of a rod of a suitable transparent crystalline material on an ultrahigh-precision lathe. During the rotation of a spindle in which the rod is mounted, a diamond tool is used to cut the rod. A computer program is used to control stepping motors that move the diamond tool, thereby controlling the shape cut by the tool. Because the shape can be controlled via software, it is possible to choose a shape designed to optimize a resonator spectrum, including, if desired, to limit the resonator to supporting a single mode. After diamond turning, a resonator can be polished to increase its Q. By virtue of its largely automated, computer-controlled nature, the process is suitable for mass production of nominally identical single-mode WGM resonators. In a demonstration of the capabilities afforded by this development, a number of WGM resonators of various designs were fabricated side by side on the surface of a single CaF2 rod (see figure).
An optical design is presented for a measurement system used to assess the impact of surface errors originating from diamond turning artifacts. Diamond turning artifacts are common by-products of optical surface shaping using the diamond turning process (a diamond-tipped cutting tool used in a lathe configuration). Assessing and evaluating the errors imparted by diamond turning (including other surface errors attributed to optical manufacturing techniques) can be problematic and generally requires the use of an optical interferometer. Commercial interferometers can be expensive when compared to the simple optical setup developed here, which is used in combination with an image-based sensing technique (phase retrieval). Phase retrieval is a general term used in optics to describe the estimation of optical imperfections or aberrations. This turnkey system uses only image-based data and has minimal hardware requirements. The system is straightforward to set up, easy to align, and can provide nanometer accuracy on the measurement of optical surface defects.
The NASA TransHab project was a flight development program of a crewed inflatable habitat designed for in-space use. Through the course of the development, several novel technologies were developed and patented by NASA. One of these patents included information regarding a custom seam stitch that was used in the TransHab restraint layer design. As the patent protection has ended, the details of the custom seam stitch are being disclosed. The seam stitch developed during the TransHab program is known as the ‘tapered diamond stitch’ and includes both a ‘single’ and ‘double’ tapered diamond pattern for ‘end termination’ and ‘continuous’ webbing components respectively. It was designed for 1-in wide Kevlar webbings with load ratings of 6,000 lbf and 12,500 lbf. The stitch pattern was designed to gradually transfer load along the length of the seam using a tapered diamond geometry. The diamond stitch has been shown in tensile testing to provide greater than 85% load strength efficiency, compared to the pristine webbing.
The high thermal conductivity, low RF loss, and inertness of diamond make it useful in traveling wave tubes operating in excess of 500 GHz. Such use requires the controlled etching of type IIA diamond to produce grating like structures tens of micrometers deep. Previous work on reactive ion etching with O2 gave etching rates on the order of 20 nm/min and poor etch selectivity between the masking material (Ni or Cr) and the diamond. An alternative approach which uses a Xe(+) beam and a reactive gas flux of NO2 in an ion-beam-assisted etching system is reported. An etching rate of 200 nm/min was obtained with an etching rate ratio of 20 between the diamond and an aluminum mask.
The production of wave-front correctors by single-point diamond turning is reported. Interferograms are shown which demonstrate excellent agreement between the diamond-turned surface and the desired surface. It is concluded from this experiment that it is now feasible by means of single-point diamond turning to make generalized wave-front control surfaces or to produce any unusual surface desired by the optical designer. The maximum departure from the nearest regular surface is set by the dynamic range and maximum diamond point acceleration permitted by the machine.
A single and dual ion beam system was used to generate amorphous carbon films with diamond like properties. A methane/argon mixture at a molar ratio of 0.28 was ionized in the low pressure discharge chamber of a 30-cm-diameter ion source. A second ion source, 8 cm in diameter was used to direct a beam of 600 eV Argon ions on the substrates (fused silica or silicon) while the deposition from the 30-cm ion source was taking place. Nuclear reaction and combustion analysis indicate H/C ratios for the films to be 1.00. This high value of H/C, it is felt, allowed the films to have good transmittance. The films were impervious to reagents which dissolve graphitic and polymeric carbon structures. Although the measured density of the films was approximately 1.8 gm/cu cm, a value lower than diamond, the films exhibited other properties that were relatively close to diamond. These films were compared with diamond like films generated by sputtering a graphite target.
The processing of interstellar dust grains by strong shock waves is studied, with the emphasis on the effects of grain-grain collisions. Such collisions provide the high pressures required to transform interstellar graphite and amorphous carbon grains into diamonds. Diamond metamorphism is as important for the destruction of such grains as vaporization and sputtering. It is calculated that about 5 percent of the C is expected to be in the form of 5-100 A diamonds in the interstellar medium. These results support the suggested interstellar origin for the recently discovered small meteoritic diamonds by providing a feasible interstellar formation mechanism.
Dense diamond-like hydrocarbon films grown at the NASA Lewis Research Center by radio frequency self bias discharge and by direct ion beam deposition were studied. A new method for categorizing hydrocarbons based on their atomic number density and elemental composition was developed and applied to the diamond-like hydrocarbon films. It was shown that the diamond-like hydrocarbon films are an entirely new class of hydrocarbons with atomic number densities lying between those of single crystal diamond and adamantanes. In addition, a major review article on these new materials was completed in cooperation with NASA Lewis Research Center personnel.
Seventeen diamond samples from diverse locations were analyzed for the contents of He, Ar, Kr, and Xe, and of their isotopes, using a Reynolds (1956) type glass mass spectrometer. The results disclosed a large spread in the He-3/He-4 ratios, ranging from values below atmospheric to close to the solar ratio. In particular, solarlike He-3/He-4 ratios were seen for an Australian colorless diamond composite and an Arkansas diamond, which also displayed solarlike neon isotopic ratios. Wide variation was also observed in the He-4/Ar-40 ratios, suggesting a complex history for the source regions and the diamond crystallization processes.
Carbon is among the most abundant elements in the universe and carbon chemistry in meteorites and comets is an important key to understanding many Solar System and interstellar processes. Yet, the mineralogical properties and interrelations between various structural forms of elemental carbon remain ambiguous. Crystalline elemental carbons include rhombohedral graphite, hexagonal graphite, cubic diamond, hexagonal diamond (i.e., lonsdaleite or carbon-2H) and chaoite. Elemental carbon also occurs as amorphous carbon and poorly graphitized (or turbostratic) carbon but of all the forms of elemental carbon only graphite is stable under physical conditions that prevail in small Solar System bodies and in the interstellar medium. The recent discovery of cubic diamond in carbonaceous chondrites and hexagonal diamond in chondritic interplanetary dust particles (IDPs) have created a renewed interest in the crystalline elemental carbons that were not formed by shock processes on a parent body. Another technique, Raman spectroscopy, confirms a widespread occurrence of disordered graphite in the Allende carbonaceous chondrite and in chondritic IDPs. Elemental carbons have also been identified by their characteristic K-edge features in electron energy loss spectra (EELS). However, the spectroscopic data do not necessarily coincide with those obtained by selected area electron diffraction (SAED). In order to interpret these data in terms of rational crystalline structures, it may be useful to consider the principles underlying electron diffraction and spectroscopic analyses. Electron diffraction depends on electron scattering, on the type of atom and the distance between atoms in a crystal lattice. Spectroscopic data are a function of the type of atom and the energy of bonds between atoms. Also, SAED is a bulk sampling technique when compared to techniques such as Raman spectroscopy or EELS. Thus, it appears that combined analyses provide contradictory results and that amorphous, or short-range ordered, carbon identified by conventional TEM imaging and SAED may show evidence for sp(3) bonds in EELS spectra. It is suggested that complex, nanometer-scale, mineralogical interrelations are common to all elemental carbons irrespective of their origin. The subsequent thermal history, or energy balance, will determine the ultimate microstructure.
A laser pulse technique to measure the thermal diffusivity of diamond films deposited on a silicon substrate is developed. The effective thermal diffusivity of diamond film on silicon was measured by observing the phase and amplitude of the cyclic thermal waves generated by the laser pulses. An analytical model is developed to calculate the effective in-plane (face-parallel) diffusivity of a two layer system. The model is used to reduce the effective thermal diffusivity of the diamond/silicon sample to a value for the thermal diffusivity and conductivity of the diamond film. Phase and amplitude measurements give similar results. The thermal conductivity of the films is found to be better than that of type 1a natural diamond.
Measurements are presented of a thin film of synthetic diamond at various wavelengths in the extreme ultraviolet. The synthetic diamond combines the transmission properties of carbon with the strength, density, and ruggedness of a natural diamond. The Extreme Ultraviolet Transmission (EUV) of a film of the synthetic diamond has shown the existence of a thin surface layer of silicon, probably in the form of silicon carbide, which is not a contaminant layer.
Polycrystalline diamond thin films have been deposited on single-crystal silicon substrates at low temperatures (not above 600 C) using a mixture of hydrogen and methane gases by high-pressure microwave plasma-assisted chemical vapor deposition. Low-temperature deposition has been achieved by cooling the substrate holder with nitrogen gas. For deposition at reduced substrate temperature, it has been found that nucleation of diamond will not occur unless the methane/hydrogen ratio is increased significantly from its value at higher substrate temperature. Selective deposition of polycrystalline diamond thin films has been achieved at 600 C. Decrease in the diamond particle size and growth rate and an increase in surface smoothness have been observed with decreasing substrate temperature during the growth of thin films. As-deposited films are identified by Raman spectroscopy, and the morphology is analyzed by scanning electron microscopy.
In measurements of the noble gases in additional samples of diamonds from the Argyle and Ellendale lamproites in Western Australia, no neon-rich stones were encountered. No neon was detected above the relatively high blank levels in the glass apparatus. White and brown diamonds showed no differences in noble gas content, nor did samples segregated by the color of long-wave UF fluorescence. The rare gas patterns in the 1.2 Ga Argyle pipe are largely consistent with implanted He-3, He-4, and fissiogenic Xe from U/Th in the matrix rock in which the diamonds have been stored for so long. These implanted species are absent in diamonds from the much younger (about 20 Ma) Ellendale pipe. Implantation formulas for several models of inhomogeneously distributed U/Th are given. Differences in He-3 content between pipe and alluvial Argyle samples are consistent with expected cosmogenic production in the latter. An expanded data base for helium and carbon isotopic data on the same samples supports a negative (He-4)-delta(C-13) correlation seen in earlier work.
Report discusses measurements of electrical conductivities of two synthetic diamond films, three synthetic diamondlike films, and two natural type IIa diamonds at temperatures from ambient to 1,200 degrees C. Measurements performed to compare electrical conductivities of state-of-the-art diamond films with those of natural insulating diamond, particularly at temperatures above 700 degrees C.
The ability to pattern ion-implantation damaged or other nondiamond carbon on a diamond substrate is useful for fabricating a variety of devices. We accomplished such patterning by an unmasked implantation into a diamond substrate followed by photolithography and a selective electrochemical etch. The use of a high resistivity medium coupled with applied biases over 50 V permitted etching without requiring contact between the substrate and an electrode. Many electrolytes gave etches that exhibit high selectivity for nondiamond carbon over both diamond and dielectrics such as photoresist. Optical, electrical, and Raman spectroscopic measurements elucidate the effects of the etch on the implanted diamond surface.