Oxidation of tungsten single crystals in the presence of a high-electric field

The effects of high-electric fields on oxidation of tungsten single crystals in 6 × 10^?4 torr of oxygen at 1200–1500 °K were studied by field emission and transmission electron microscopy. Exposure of field emitters to oxygen in the absence of a field resulted in the build-up of emitter tips. Oxidation under the application of a negative or positive field, on the other hand, involved plane faceting and formation of oxide crystallites. Plane faceting was recognized to occur on the {111} and the {112} regions, showing the facetings of the {111} and the {112} planes into the {110} planes, whereas, crystallite formation seemed to take place selectively on the {100} regions. It was suggested by field emission microscopy that negative fields have an additional effect which causes the growth of an oxide crystal on the (110) plane. Transmission electron microscopy of an emitter oxidized in a negative field actually revealed a tiny oxide crystal with a size of ～ 300 Å grown on the developed (110) plane. The crystal exhibited a triangular shadow image strongly indicating an external pyramid-like form.     

Direct observation of the atomic structure of W {100} surfaces

Fully resolved atomic images of the W {100} plane are obtained with the field ion microscope at 21°K. The image structure is consistent with the (1 × 1) structure. If shifts of atoms in the 〈110〉 directions parallel to the plane have occurred as derived from LEED investigations in the temperature range of 100–370°K, then the shifts at 21°K are too small to be observed in the FIM.     

Mechanical behavior of poly(ethyleoe terephthalate) at cryogenic temperatures

The mechanical behavior of poly(ethylene terephthalate) (PET) was studied at temperatures from 4 to 300°K with a free oscillating torsion pendulum and an Instron tester.

Torsion pendulum data show the presence of relaxation maxima below 80°K. Noncrystalline specimens show a small peak at 48°K (δ) and a shoulder at 8-12° K (?). A peak at 20° K is observed in crystalline samples, both oriented and unoriented. In addition drawn specimens show a pronounced peak at 48° K and the assymmetric maximum in the 100-240° K region is split into two peaks. The logarithmic decrement in the β-loss region decreases with increasing crystallinity and orientation, while the cryogenic loss peaks increase in intensity.

Tensile tests with biaxially oriented and heat-set films show a twofold increase in elastic modulus and a tenfold increase in toughness at cryogenic temperatures when compared with “amorphous” PET.     

Laser Light and X-Ray Diffraction Studies of Oriented Isotactic Polypropylene (iPP) Prepared by Temperature Slope Crystallization

Isotactic polypropylene (iPP) film was melt-crystallized in a temperature gradient. The iPP film showed well oriented α- and β-crystalline textures along the gradient. The crystalline structure, phase transition boundary and lamellar twisting were examined by X-ray diffraction and laser light diffraction (LLD). On the α-β boundary, LLD shows a sharp streak perpendicular to the boundary, where the a-axis of the β-crystal is oriented perpendicular to the temperature gradient. Apart from the boundary, the a-axis of the β-crystal becomes parallel to the gradient. The β-crystal shows lamellar twisting with a pitch of 200 μm at room temperature. When heated the β-crystal, the lamellar distance of 295Å at room temperature decreases to 285Å at 80–100°C and then increases to more than 300Å above 120°C. During the heating, the value of the twist period increases from 200 to 210 μm at 90–100°C, and then to above 224 μm at 140°C. The increase of the twist period is related to the increasing crystalline thickness of the β-lamellae.     

Magnetic properties of ultrathin Ni films

The magnetic properties of Au/Ni/Si(100) films with Ni thicknesses of 8–200 Å are studied at T=77 K using a scanning magnetic microscope with a thin-film high-temperature dc SQUID. It is found that the Ni films, with an area of 0.6×0.6 mm, which are thicker than 26 Å have a single-domain structure with the magnetic moment oriented in the plane of the film and a saturation magnetization close to 0.17 MA/m. For films less than 26 Å thick, the magnetization of the film is found to drop sharply.     

Dependence of the specific heat of a La1.85Sr0.15CuO4 superconducting single crystal on the magnetic field direction in the a-b plane

The low-temperature specific heat of a La_1.85Sr_0.15CuO₄ superconducting single crystal was investigated in magnetic fields up to 8 T and with four orientations — in the a-b plane (along the (100) and (110) directions) and at angles of 45° and 90° with respect to the a-b plane (along the (103) and (001) directions). Anisotropy was observed in the field dependence of the specific heat in the a-b plane. The specific heat was found to be minimum with the field oriented in the direction of the a axis and maximum with the field oriented in a direction making an angle of 45° with the a axis. This can be explained by the anisotropy of the energy gap, whose minimum lies along the (110) direction. For all orientations of the magnetic field the specific heat of the mixed state at low temperatures is a nonlinear function of the magnetic field strength. Pis’ma Zh. éksp. Teor. Fiz. 66, No. 11, 683–687 (10 December 1997)     

Deformation and annealing behavior. II. Thick polyethylene terephthalate films

Thick (5-30 mil) samples of polyethylene terephthalate (PET), drawn uniaxially and biaxially followed by thermal crystallization, were studied by replication electron microscopy and wide- and small-angle X-rays. Deformation of gold-decorated samples indicated that aggregates on the 200–500 Å scale move as units during deformation. Thermal crystallization of both uniaxially and biaxially drawn samples occurred with the formation of coarse 200–500 Å nodular aggregates, which, in turn, may consist of the 75–100 Å nodules observed by Yeh and Geil. At annealing temperatures above 180° C, fibrillar lamellae are formed, arranged perpendicular to the draw direction in uniaxially drawn samples and at random in biaxially drawn samples. Small-angle photographs and pole figures of uniaxially drawn and annealed samples can be explained in terms of a toroidal arrangement of poles centered about the draw direction.     

Versuch einer quantitativen Erfassung der Textur von Gold-Aufdampfschichten

The fiber texture of evaporated gold films is investigated by a registration technique inside a Siemens Elmiskop I. The intensity of electron diffraction is measured along the circumference of the Debye-Scherrer ring. The thickness of the films varies in the range 50 to 700 Å and the glass substrate temperature from room temperature to 400°C. In all films we found a (111) fiber texture. Subsidiary maxima of a (511) texture are contributed to the formation of microtwins. For comparison of the texture a quantityT is introduced.T has a strong relation to the electron microscopical structure of the films. Layers with island structure and with small crystals at low substrate temperatures exhibit only very small values ofT. The textureT increases with increasing recrystallisation, (111) oriented crystals having the largest growing rate in the layer plane.     

Crystal habits of Pd and Pt particles: Nature of surface sites

Morphology of small Pd and Pt crystallites prepared by vacuum condensation has been studied by electron microscopy so as to determine the surface sturcture. A high resolution dark field technique is used to obtain the crystallite shape. It was found that in a range of size 60–200 Å most crystallites are bordered by incomplete (111) layers which give a large number of surface “B₅ sites”.     

Angular dependence of the in-plane magnetization of (100) Cu/Ni/Cu structures

(100) Cu/Ni/Cu sandwich structures have been deposited on (100) Si using the (100) Cu epitaxially grown as the seed layer. The in-plane epitaxial relation between the metal films and Si allows the study of angular dependence of the magnetization for the field parallel to the film plane. Keeping the Cu layers at 1000 Å each and varying the Ni layers between 50 and 1000 Å, the magnetization along the [110] edge is larger than that along the [100] one. This is observed for both structures with a Ni thickness of 1000 and 500 Å, respectively. For the thinner Ni layers, the angular dependence is interfered by the reversal in magnetic anisotropy reported earlier. For such structures, a squared hysteresis loop is observed for the field perpendicular to the film plane, whereas one with little loop is observed for the in-plane magnetization. The angular dependence observed for the 1000 and 500 Å Ni films is the same as that of single crystal Ni. The (100) Cu/Ni/Cu films thus grown can be used for other magnetic measurements in the exploration of two-dimensional magnetism with controlled orientations.     

Magnetically induced spin-rotation transition in iron-garnet films with canted-phase anisotropy

Epitaxial iron-garnet films exhibiting canted-phase and easy-plane anisotropies, with crystallographic (111) surface orientation are investigated by magnetooptical and inductive frequency methods. It is shown that four types of domain structure exist in the films. When the magnetization of the films is reversed by a static magnetic field oriented at various angles to the normal to the plane, anomalous behavior of the magnetic susceptibility is observed in the interval of magnetic-field orientation angles from 0.3° to 1.5°. Fiz. Tverd. Tela (St. Petersburg) 39, 1415–1420 (August 1997)     

Chemisorption studies on cobalt single crystal surfaces: I. Carbon monoxide on Co(0001)

The chemisorption of CO on Co(0001) and on a polycrystalline specimen has been studied by LEED, Auger spectroscopy, and thermal desorption measurements. Annealing of the polycrystal was found to result in a surface dominated by crystallites of (0001) orientation in the surface plane, along with a few (101̄2) oriented crystallites. CO adsorbs on the clean surface at 300 K with an initial sticking probability of 0.9 and the system follows precursor state kinetics. The saturation coverage under UHV conditions corresponds to a well-ordered (√3 × √3)R30° structure; with P_CO>5 × 10^-9 a uniform compression of the adlayer takes place and a (√7 × √7)R19.2° structure begins to form. Models are proposed for these two ordered phases which are in agreement with the observed relative coverage data and the appearance of the corresponding desorption spectra. The desorption enthalpy of CO at low coverages is 103 ± 8 kJmol^-1, and a fairly sharp fall in this enthalpy occurs for coverages $\text{>}\text{1}\text{3}$. In many respects, the system's behaviour closely resembles that of Ni(111)-CO. Oxygen contamination leads to the appearance of a strongly adsorbed CO state with a desorption enthalpy of ~170 kJmol^-1. This is reminiscent of a strongly adsorbed non-dissociated state of CO on Ru(101̄1) which occurs under similar conditions.     

Superparamagnetism and magnetic granulometry of vitroceramics containing iron-lithium ferrite

Magnetic properties of lithium ferrite crystallites distributed in a glassy matrix vary with their average size d: (1) d ? 100 Å: superparamagnetism d and the limits of the distribution have been calculated by fitting magnetisation curves vs applied field. (2) d ? 150 Å: ferrimagnetism with a hysteresis loop maximum for the monodomain size (260 ± 40 Å). (3) 100 ? d ? 150 Å: superposition of the two preceding phenomena.     

Mechanical Behavior of Bulk Poly(Ethylene Terephthalate) Subjected to Simple Shear

Abstract

Mechanical behavior of bulk semicrystalline poly(ethylene terephthalate) (PET) processed through simple shear is investigated. The equal channel angular extrusion (ECAE) process was used to achieve the simple shear condition. The PET samples were processed in one and two ECAE passes in the same direction, with the sample rotated 180° about the extrusion axis for the second pass. Microstructural features at the nanometer and micrometer scales were studied by small‐angle x‐ray scattering (SAXS) and scanning electron microscopy (SEM). SAXS results showed that at the nanometer scale, two types of lamellar orientations are induced in both samples, but with different extents of orientation. In the ECAE‐oriented PET structures on the micrometer scale, as revealed by SEM, are well‐defined macrofibrils. However, the fibrillar structures in the sample extruded once are more oriented than those in the sample extruded twice. Fractography investigations suggest that the ECAE‐induced fibrillar structure and stretched amorphous chains are responsible for the change in mechanical properties.     

Electron microscopical study of pyro-carbon microneedles grown by high field pyrolysis

Investigations with transmission electron microscopy and selected area electron diffraction demonstrated that high field polymerization products grown at room temperature with benzonitrile are of needle shape and have an amorphous structure. High field pyrolyzation products which originated at high temperatures (1200° C) display a morphologically similar, but mechanically more stable composition as well as a larger number of needles per unit area. Their structure corresponds to an arrangement of layers of graphitelike regions concentric to the needle axis. According to the evaluation of the electron diffraction diagrams obtained, it was possible to image directly in the electron microscope the curved lattice planes of the high field pyrolyzation products, in close agreement with the net plane distance of the 001 lattice planes of graphite (3.35 Å).     

X-ray crystallographic study of solid-state polymerization of trioxane and tetraoxymethylene

An X-ray study has been applied to clarify the relationship between crystal structures and crystal orientations of tetraoxymethylene and polyoxymethylene obtained by solid- state polymerization of tetraoxymethylene. The polyoxymethylene crystal obtained by the solidstate polymerization of a tetraoxymethylene single crystal was found to be definitely oriented with respect to the original tetraoxymethylene single crystal without any aftertreatment; i.e., the polymer chain (the c-axis) is parallel to the b-axis of tetraoxymethylene and the a-axis of polyoxymethylene coincides to the c-axis of tetraoxymethylene.

In addition to the main orientation, other preferred crystalline orientations (“twin structure”) of polyoxymethylene were observed in polymers polymerized at lower temperatures (60-80°C); i.e., the polymer chains are parallel to either the [100], [001], or [101] direction of the original tetraoxymethylene crystal, though the amount of such oriented crystallites is small. The twin structure is different from that of polyoxymethylene obtained from trioxane. This difference is due to the crystal structures of these original materials; tetraoxymethylene occurs in the monoclinic system, while trioxane belongs to the trigonal system, as does polyoxymethylene. These characteristic orientations are explained in terms of the molecular arrangements in the crystals of the original materials.     

Size effect of the longitudinal magnetoresistance of thin films of n- type Ge

In a study of the longitudinal magnetoresistance as a function of the magnetic field in samples of n-type Ge of various thicknesses at 300°K and 77°K, the surface of the samples was oriented parallel to the (001) plane. The directions of the current and the magnetic field were along either the <100> direction or the <110> direction. As the thickness of the samples was reduced, regardless of the orientation of the current and the magnetic field with respect to the crystallographic directions, a decrease was observed in the magnetoresistance over the entire range of magnetic fields studied, 1–280 kOe. The experimental results are attributed to a screening-length size effect and to “sliding” orbits in the enriched surface layers, which lead to an increase in the electron mobility in a strong magnetic field.     

Comparative AES and RHEED study of the formation of Pd silicide on clean and oxide covered Si(100) and (111) surfaces

The formation and epitaxial orientation of Pd silicide on clean and native oxide covered Si(100) and (111) surfaces was studied by Auger electron spectroscopy (AES) and reflection high energy electron diffraction (RHEED). Pd was vapor deposited in UHV on to the substrates up to thicknesses of about 6 nm. On clean Si substrates, ultra-thin Pd deposits reacted to form Pd₂Si already at room temperature, as detected by a characteristic splitting of the Si LVV Auger peak. However, a polycrystalline structure with very small crystallite sizes was indicated by diffuse ring patterns in RHEED. When the initial thickness of the Pd deposit exceeded about 3 nm, the diffraction ring pattern of unreacted metal developed. During annealing of room temperature deposits of Pd, the (100) and (111) substrates behaved differently. Larger crystallites formed on Si(100), but the films remained polycrystalline, though textured. On Si(111), virtually perfect epitaxial re-orientation of the silicide was found. When the substrates were initially covered with native oxide of about 2 nm thickness, silicide formation started at about 200°C, resulting in polycrystalline, but strongly textured Pd₂Si. Upon further annealing at temperatures up to 600°C, an additional phase of epitaxially oriented Pd₂Si developed on Si(111), similar to that on clean Si(100). In all experiments, extended annealing at temperatures above 250°C caused segregation of Si to the surface. This was accompanied by the development of an additional peak in the Auger electron spectra at about 313 eV, which we assign to a plasmon loss of δE = 17 eV in the Si overlayer, being excited by Pd Auger electrons of energy 330 eV.     

Solid-phase synthesis of L1<Subscript>0</Subscript>-FePd(001) epitaxial thin films: Structural transformations and magnetic anisotropy

The solid-phase synthesis of the L1₀-FePd magnetically hard phase in Fe(001)/Pd(001) epitaxial films has been experimentally investigated. The formation of three types of L1₀-FePd ordered crystallites whose c axes coincide with the 〈100〉 directions of the MgO(001) substrate begins at the Fe/Pd interface at a temperature of 450°C. After an increase in the annealing temperature to 500°C, structural rearrangement occurs and gives rise to the predominant growth of L1₀-FePd crystallites with the c axis perpendicular to the film plane. After 10-h annealing, the fraction of such crystallites becomes dominant, leading to large perpendicular anisotropy. The first magnetocrystalline-anisotropy constant of the L1₀-FePd phase has been determined and the second constant has been estimated. It has been shown that magnetic anisotropy in the L1₀-FePd(001) basal plane cannot be described by the biaxial anisotropy of the tetragonal crystal. The annealing above 500°C results in the evolution of L1₀-FePd to a disordered cubic phase.     

Migration brownienne de cristallites sur une surface et relation avec l'épitaxie: IV. Mobilité de cristallites sur une surface: Décoration de gradins monoatomiques de surface

The influence of a monoatomic step on the brownian movement of small gold crystallites on (100) KCl has been studied. It is experimentally demonstrated that: (a) the crystallites migrate along a step; (b) a gold decorated step provides an effective barrier for the migrating crystallites on the plane surface; (c) a non-decorated step may effectively capture the incoming crystallites.