Nearly Perfect Electrical Activation Efficiencies from Silicon-Implanted Al<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>Ga<Subscript>1−<Emphasis Type="Italic">x</Emphasis></Subscript>N with High Aluminum Mole Fraction

Electrical activation studies of Al _x Ga_1−x N (x = 0.45 and 0.51) implanted with Si for n-type conductivity have been made as a function of ion dose and anneal temperature. Silicon ions were implanted at 200 keV with doses ranging from 1 × 10¹⁴ cm⁻² to 1 × 10¹⁵ cm⁻² at room temperature. The samples were subsequently annealed from 1150°C to 1350°C for 20 min in a nitrogen environment. Nearly 100% electrical activation efficiency was successfully obtained for the Si-implanted Al_0.45Ga_0.55N samples after annealing at 1350°C for doses of 1 × 10¹⁴ cm⁻² and 5 × 10¹⁴ cm⁻² and at 1200°C for a dose of 1 × 10¹⁵ cm⁻², and for the Al_0.51Ga_0.49N implanted with silicon doses of 1 × 10¹⁴ cm⁻² and 5 × 10¹⁴ cm⁻² after annealing at 1300°C. The highest room-temperature mobility obtained was 61 cm²/V s and 55 cm²/V s for the low-dose implanted Al_0.45Ga_0.55N and Al_0.51Ga_0.49N, respectively, after annealing at 1350°C for 20 min. These results show unprecedented activation efficiencies for Al _x Ga_1−x N with high Al mole fractions and provide suitable annealing conditions for Al _x Ga_1−x N-based device applications.     

Exfoliation and blistering of Cd<Subscript>0.96</Subscript>Zn<Subscript>0.04</Subscript>Te substrates by ion implantation

As part of a series of wafer bonding experiments, the exfoliation/blistering of ion-implanted Cd_0.96Zn_0.04Te substrates was investigated as a function of postimplantation annealing conditions. (211) Cd_0.96Zn_0.04Te samples were implanted either with hydrogen (5×10¹⁶ cm⁻²; 40–200 keV) or co-implanted with boron (1×10¹⁵ cm⁻²; 147 keV) and hydrogen (1–5×10¹⁶ cm⁻²; 40 keV) at intended implant temperatures of 253 K or 77 K. Silicon reference samples were simultaneously co-implanted. The change in the implant profile after annealing at low temperatures (<300°C) was monitored using high-resolution x-ray diffraction, atomic force microscopy (AFM), and optical microscopy. The samples implanted at the higher temperature did not show any evidence of blistering after annealing, although there was evidence of sample heating above 253 K during the implant. The samples implanted at 77 K blistered at temperatures ranging from 150°C to 300°C, depending on the hydrogen implant dose and the presence of the boron co-implant. The production of blisters under different implant and annealing conditions is consistent with nucleation of subsurface defects at lower temperature, followed by blistering/exfoliation at higher temperature. The surface roughness remained comparable to that of the as-implanted sample after the lower temperature anneal sequence, so this defect nucleation step is consistent with a wafer bond annealing step prior to exfoliation. Higher temperature anneals lead to exfoliation of all samples implanted at 77 K, although the blistering temperature (150–300°C) was a strong function of the implant conditions. The exfoliated layer thickness was 330 nm, in good agreement with the projected range. The “optimum” conditions based on our experimental data showed that implanting CdZnTe with H⁺ at 77 K and a dose of 5×10¹⁶/cm² is compatible with developing high interfacial energy at the bonded interface during a low-temperature (150°C) anneal followed by layer exfoliation at higher (300°C) temperature.     

Electrical Activation Studies of Silicon-Implanted Al<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>Ga<Subscript>1−<Emphasis Type="Italic">x</Emphasis></Subscript>N with Aluminum Mole Fraction of 11% to 51%

Electrical activation studies of Si-implanted Al _x Ga_1−x N with an Al mole fraction of 11% to 51% have been carried out as a function of ion dose and annealing temperature. The Al _x Ga_1−x N samples were implanted at room temperature with Si ions at 200 keV in doses ranging from 1 × 10¹⁴ cm⁻² to 1 × 10¹⁵ cm⁻², and subsequently annealed from 1100°C to 1350°C for 20 min in a nitrogen environment. The maximum electrical activation efficiencies for the Al _x Ga_1−x N samples with an Al mole fraction less than 40% were obtained for samples implanted with the highest Si dose of 1 × 10¹⁵ cm⁻². On the other hand, for the Al _x Ga_1−x N samples with an Al mole fraction more than 40%, nearly perfect activation efficiencies of 99% and 100% were obtained for the samples implanted with the lowest Si dose of 1 × 10¹⁴ cm⁻². The mobility of the Si-implanted Al _x Ga_1−x N samples increased with increasing annealing temperature in spite of the increased number of ionized donors and thus increased impurity scattering, indicating that a greater amount of lattice damage is being repaired with each successive increase in annealing temperature. These results provide suitable annealing conditions for Si-implanted Al _x Ga_1−x N-based devices with an Al mole fraction from 11% to 51%.     

Effect of Rapid Thermal Annealing on Sputtered CaCu<Subscript>3</Subscript>Ti<Subscript>4</Subscript>O<Subscript>12</Subscript> Thin Films

Calcium copper titanium oxide (CaCu₃Ti₄O₁₂, abbreviated to CCTO) films were deposited on Pt/Ti/SiO₂/Si substrates at room temperature (RT) by radiofrequency magnetron sputtering. As-deposited CCTO films were treated by rapid thermal annealing (RTA) at various temperatures and in various atmospheres. X-ray diffraction patterns and scanning electron microscope (SEM) images demonstrated that the crystalline structures and surface morphologies of CCTO thin films were sensitive to the annealing temperature and ambient atmosphere. Polycrystalline CCTO films could be obtained when the annealing temperature was 700°C in air, and the grain size increased signifi- cantly with annealing in O₂. The 0.8-μm CCTO thin film that was deposited at RT for 2 h and then annealed at 700°C in O₂ exhibited a high dielectric constant (ε′) of 410, a dielectric loss (tan δ) of 0.17 (at 10 kHz), and a leakage current density (J) of 1.28 × 10⁻⁵ A/cm² (at 25 kV/cm).     

Crystallization of Amorphous Si<Subscript>0.6</Subscript>Ge<Subscript>0.4</Subscript> Nanoparticles Embedded in SiO<Subscript>2</Subscript>: Crystallinity Versus Compositional Stability

Si_0.6Ge_0.4 nanocrystals, of diameter <5 nm, embedded in SiO₂ in the form of single layers (2.1 × 10¹² nanoparticles cm^–2) and five-period multilayers (above 10¹³ nanoparticles cm^–2) have been fabricated using a low-thermal-budget process consisting of deposition by low-pressure chemical vapor deposition and crystallization by rapid thermal annealing at several temperatures and for different times. The crystallization process was monitored by Raman spectroscopy and transmission electron microscopy. The loss of integrity and compositional changes of the nanoparticles during the annealing process were characterized by Rutherford backscattering spectrometry. During the annealing process, crystallization and Ge out-diffusion have been observed to compete with each other. Annealing of samples with nanoparticles of 4.6 nm diameter at low temperature (750°C) yields poor crystallization of the nanoparticles and causes the Ge to leave them by a pure diffusive mechanism, thus destroying their integrity. At higher temperatures (≥800°C), crystallization takes place in a short period of time (<30 s) and diffusion from the crystallized material is initially hindered. For samples with nanoparticles of 3.3 nm diameter, partial crystallization is detected at 800°C and 900°C and the crystalline quality is improved in both cases as the annealing time increases. Also, the detection capabilities of the Raman spectroscopy system for the detection of a certain density of SiGe nanocrystals of given diameter and composition have been explored and the lower limit estimated.     

Effect of Proton Irradiation on Interface State Density in Sc<Subscript>2</Subscript>O<Subscript>3</Subscript>/GaN and Sc<Subscript>2</Subscript>O<Subscript>3</Subscript>/MgO/GaN Diodes

Proton irradiation of Sc₂O₃/GaN and Sc₂O₃/MgO/GaN metal-oxide semiconductor diodes was performed at two energies, 10 MeV and 40 MeV, and total fluences of 5 × 10⁹ cm⁻², corresponding to 10 years in low-earth orbit. The proton damage causes a decrease in forward breakdown voltage and a flat-band voltage shift in the capacitance-voltage characteristics, indicating a change in fixed oxide charge and damage to the dielectric. The interface state densities after irradiation increased from 5.9 × 10¹¹ cm⁻² to 1.03 × 10¹² cm⁻² in Sc₂O₃/GaN diodes and from 2.33 × 10¹¹ to 5.3 × 10¹¹ cm⁻² in Sc₂O₃/MgO/GaN diodes. Postannealing at 400°C in forming gas recovered most of the original characteristics but did increase the interfacial roughness.     

Thermoelectric Performance of Zn and Nd Co-doped In<Subscript>2</Subscript>O<Subscript>3</Subscript> Ceramics

Polycrystalline In₂O₃ ceramics co-doped with Zn and Nd were prepared by the spark plasma sintering (SPS) process, and microstructure and thermoelectric (TE) transport properties of the ceramics were investigated. Our results indicate that co-doping with Zn²⁺ and Nd³⁺ shows a remarkable effect on the transport properties of In₂O₃-based ceramics. Large electrical conductivity (~130 S cm⁻¹) and thermopower (~220 μV K⁻¹) can be observed in these In₂O₃-based ceramic samples. The maximum power factor (PF) reaches 5.3 × 10⁻⁴ W m⁻¹ K⁻² at 973 K in the In_1.92Nd_0.04Zn_0.04O₃ sample, with a highest ZT of ~0.25.     

Vapor Annealing as a Post-Processing Technique to Control Carrier Concentrations of Bi<Subscript>2</Subscript>Te<Subscript>3</Subscript> Thin Films

This article demonstrates that carrier concentrations in bismuth telluride films can be controlled through annealing in controlled vapor pressures of tellurium. For the bismuth telluride source with a small excess of tellurium, all the films reached a steady state carrier concentration of 4 × 10¹⁹ carriers/cm³ with Seebeck coefficients of −170 μV K⁻¹. For temperatures below 300°C and for film thicknesses of 0.4 μm or less, the rate-limiting step in reaching a steady state for the carrier concentration appeared to be the mass transport of tellurium through the gas phase. At higher temperatures, with the resulting higher pressures of tellurium or for thicker films, it was expected that mass transport through the solid would become rate limiting. The mobility also changed with annealing, but at a rate different from that of the carrier concentration, perhaps as a consequence of the non-equilibrium concentration of defects trapped in the films studied by the low temperature synthesis approach.     

Vanadium-based ohmic contacts to n-type Al<Subscript>0.6</Subscript>Ga<Subscript>0.4</Subscript>N

Four vanadium-based contacts to n-type Al_0.6Ga_0.4N were compared in this work. Both V/Al/Pd/Au and V/Al/V/Au contacts with optimized layer thicknesses provided lower specific-contact resistances than did the previously reported V/Al/Pt/Au ohmic contact. Specific contact resistances of the V/Al/Pd/Au (15 nm/85 nm/20 nm/95 nm) and V/Al/V/Au (15 nm/85 nm/20 nm/95 nm) contacts were 3×10⁻⁶ Ω·cm² and 4×10⁻⁶ Ω·cm², respectively. On the other hand, an analogous V/Al/Mo/Au contact never became ohmic, even after it was annealed at 900°C for 30 sec. Compared to the V/Al/Pd/Au contact, the V/Al/V/Au contact required a less severe annealing condition (30 sec at 700°C instead of 850°C). The V/Al/V/Au contact also provided a smoother surface, with a root-mean-square (RMS) roughness of 39 nm.     

Influence of Surface Treatment and Annealing Temperature on the Formation of Low-Resistance Au/Ni Ohmic Contacts to <Emphasis Type="Italic">p</Emphasis>-GaN

We have studied the influence of surface treatment and annealing temperature on the specific contact resistance of Au/Ni ohmic contacts to p-GaN with hole concentrations in the range of 10¹⁶ cm⁻³ to 10¹⁸ cm⁻³. The sample with a hole concentration of 1 × 10¹⁸ cm⁻³, treated with the surface treatment HCl:H₂O = 3:1 solution and annealed at 500°C in a 90% N₂ and 10% O₂ atmosphere, yielded the lowest specific contact resistance of ~4 × 10⁻⁵ Ω cm² and ~2 × 10⁻⁷ Ω cm² at room temperature and at 150°C, respectively. To investigate the roles of interdiffusion between layer interfaces and the formation of NiO and nickel gallides, we examined the metallization stacks before and after annealing using high-resolution x-ray diffraction. We conclude that the nickel-gallide formation and the deterioration of the NiO layer are together responsible for the large deviation in contact resistances observed for samples annealed at various temperatures.     

Light-emitting Si nanostructures formed in SiO<Subscript>2</Subscript> on irradiation with swift heavy ions

SiO₂ layers containing implanted excess Si are irradiated with Xe ions with an energy of 130 MeV and doses of 3 × 10¹²–10¹⁴ cm⁻². In the samples irradiated with a dose of 3 × 10¹² cm⁻², ∼10¹² cm⁻² segregated clusters 3–4 nm in dimension are detected by transmission electron microscopy. With increasing dose, the dimensions and number of these clusters increase. In the photoluminescence spectrum, a 660- to 680-nm band is observed, with the intensity dependent on the dose. After passivation of the sample with hydrogen at 500°C, the band disappears, but a new ∼780-nm band typical of Si nanocrystals becomes evident. On the basis of the entire set of data, it is concluded that the 660- to 680-nm band is associated with imperfect Si nanocrystals grown in the tracks of Xe ions due to high ionization losses. The nonmonotonic dependence of the photoluminescence intensity on the dose is attributed to the difference between the diameters of tracks and the diameters of the displacements’ cascades responsible for defect formation.     

Thermoelectric Properties of Ag-doped Mg<Subscript>2</Subscript>Ge Thin Films Prepared by Magnetron Sputtering

Silver doped p-type Mg₂Ge thin films were grown in situ at 773 K using magnetron co-sputtering from individual high-purity Mg and Ge targets. A sacrificial base layer of silver of various thicknesses from 4 nm to 20 nm was initially deposited onto the substrate to supply Ag atoms, which entered the growing Mg₂Ge films by thermal diffusion. The addition of silver during film growth led to increased grain size and surface microroughness. The carrier concentration increased from 1.9 × 10¹⁸ cm⁻³ for undoped films to 8.8 × 10¹⁸ cm⁻³ for the most heavily doped films, but it did not reach saturation. Measurements in the temperature range of T = 200–650 K showed a positive Seebeck coefficient for all the films, with maximum values at temperatures between 400 K and 500 K. The highest Seebeck coefficient of the undoped film was 400 μV K⁻¹, while it was 280 μV K⁻¹ for the most heavily doped film at ∼400 K. The electrical conductivity increased with silver doping by a factor of approximately 10. The temperature effects on power factors for the undoped and lightly doped films were very limited, while the effects for the heavily doped films were substantial. The power factor of the heavily doped films reached a non-optimum value of ∼10⁻⁵ W cm⁻¹ K⁻² at 700 K.     

Efficient Outdiffusion of Hydrogen from Mg-Doped Nitrides by NF<Subscript>3</Subscript> Annealing

High concentration (more than 1 × 10¹⁸ cm⁻³) of hydrogen atoms remaining in Mg-doped GaN epitaxial layers grown by metalorganic chemical vapor deposition even after conventional annealing in N₂ ambient could induce degradation in GaN-based devices containing Mg-doped layers. In this study, by annealing Mg-doped nitrides in NF₃ ambient, we successfully reduced residual hydrogen below mid-10¹⁷ cm⁻³, which is much smaller than by N₂ annealing. NF₃ annealing enhances outdiffusion of hydrogen from the bulk, which is possibly because the nitrogen and fluorine radicals decomposed from NF₃ accelerate desorption of hydrogen adatoms from the surface. The proposed method for Mg activation would improve the reliability of GaN-based light-emitting diodes and laser diodes.     

Synthesis and Electronic Properties of the Misfit Layer Compound [(PbSe)<Subscript>1.00</Subscript>]<Subscript>1</Subscript>[MoSe<Subscript>2</Subscript>]<Subscript>1</Subscript>

An ultralow-thermal-conductivity compound with the ideal formula [(PbSe)_1.00]₁[MoSe₂]₁ has been successfully crystallized across a range of compositions. The lattice parameters varied from 1.246 nm to 1.275 nm, and the quality of the observed 00ℓ diffraction patterns varied through the composition region where the structure crystallized. Measured resistivity values ranged over an order of magnitude, from 0.03 Ω m to 0.65 Ω m, and Seebeck coefficients ranged from −181 μV K⁻¹ to 91 μV K⁻¹ in the samples after the initial annealing to form the basic structure. Annealing of samples under a controlled atmosphere of selenium resulted in low conductivities and large negative Seebeck coefficients, suggesting an n-doped semiconductor. Scanning transmission electron microscopy cross-sections confirmed the interleaving of bilayers of PbSe with Se-Mo-Se trilayers. High-angle annular dark-field images revealed an interesting volume defect, where PbSe grew through a region where a layer of MoSe₂ would be expected in the perfect structure. Further studies are required to correlate the density of these defects with the observed electrical properties.     

Development of (Bi,Sb)<Subscript>2</Subscript>(Te,Se)<Subscript>3</Subscript>-Based Thermoelectric Modules by a Screen-Printing Process

In major applications, optimal power will be achieved when thermoelectric films are at least 100 μm thick. In this paper we demonstrate that screen-printing is an ideal method to deposit around 100 μm of (Bi,Sb)₂(Te,Se)₃-based films on a rigid or flexible substrate with high Seebeck coefficient value (90 μV K⁻¹ to 160 μV K⁻¹) using a low-temperature process. Conductive films have been obtained after laser annealing and led to acceptable thermoelectric performance with a power factor of 0.06 μW K⁻² cm⁻¹. While these initial material properties are not at the level of bulk materials, the complete manufacturing process is cost-effective, compatible with large surfaces, and affords a mass-production technique.     

Preparation of Well-Tiled <Emphasis Type="Italic">γ</Emphasis>-Na<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>Co<Subscript>2</Subscript>O<Subscript>4</Subscript> by a Novel and Simple Sodium Alginate Gel Method and Its Electrical Properties

In this paper, a novel and simple sodium alginate (SA) gel method was developed to prepare γ-Na _x Co₂O₄. This method involved the chemical gelling of SA in the presence of Co²⁺ ions by cross-linking. After calcining at 700°C to 800°C, single-phase γ-Na _x Co₂O₄ crystals were obtained. The arrangement of about 1 μm to 4 μm flaky particles exhibited a well-tiled structure along the plane direction of the flaky particles. SA not only acted as the control agent for crystal growth, but also provided a Na source for the γ-Na _x Co₂O₄ crystals. The electrical properties of γ-Na _x Co₂O₄ ceramics prepared via ordinary sintering after cold isostatic pressing were investigated. The Seebeck coefficient and power factor of the bulk material were 177 μV K⁻¹ and 4.3 × 10⁻⁴ W m⁻¹ K⁻² at 850 K, respectively.     

Thermoelectric Properties of Zr<Subscript>3</Subscript>Mn<Subscript>4</Subscript>Si<Subscript>6</Subscript> and TiMnSi<Subscript>2</Subscript>

The Seebeck coefficient, electrical resistivity, and thermal conductivity of Zr₃Mn₄Si₆ and TiMnSi₂ were studied. The crystal lattices of these compounds contain relatively large open spaces, and, therefore, they have fairly low thermal conductivities (8.26 Wm⁻¹ K⁻¹ and 6.63 Wm⁻¹ K⁻¹, respectively) at room temperature. Their dimensionless figures of merit ZT were found to be 1.92 × 10⁻³ (at 1200 K) and 2.76 × 10⁻³ (at 900 K), respectively. The good electrical conductivities and low Seebeck coefficients might possibly be due to the fact that the distance between silicon atoms in these compounds is shorter than that in pure semiconductive silicon.     

Crystallization behavior and ferroelectric properties of PbTiO<Subscript>3</Subscript>/Ba<Subscript>0.85</Subscript>Sr<Subscript>0.15</Subscript>TiO<Subscript>3</Subscript>/PbTiO<Subscript>3</Subscript> sandwich thin film on Pt/Ti/SiO<Subscript>2</Subscript>/Si substrates

A PbTiO₃/Ba_0.85Sr_0.15TiO₃/PbTiO₃ (PT/BST15/PT) sandwich thin film has been prepared on Pt/Ti/SiO₂/Si substrates by an improved sol-gel technique. It is found that such films under rapid thermal annealing at 700°C crystallize more favorably with the addition of a PbTiO₃ layer. They possess a pure, perovskite-phase structure with a random orientation. The polarization-electric field (P-E) hysteresis loop and current-voltage (I-V) characteristic curves reveal that a PT/BST15/PT film exhibits good ferroelectricity at room temperature. However, no sharp peak, only a weak maximum, is observed in the curves of the dielectric constant versus temperature. The dielectric constant, loss tangent, leakage current density at 20 kV/cm, remnant polarization, and coercive field of the PT/BST15/PT film are 438, 0.025, 1.3 × 10⁻⁶ Acm⁻², 2.46 μCcm⁻², and 41 kVcm⁻¹, respectively, at 25°C and 10 kHz. The PT/BST15/PT film is a candidate material for high sensitivity elements for uncooled, infrared, focal plane arrays (UFPAs) to be used at near ambient temperature.     

Electronic properties and deep traps in electron-irradiated <Emphasis Type="Italic">n</Emphasis>-GaN

The study is concerned with the effect of electron irradiation (with the energies E = 7 and 10 MeV and doses D = 10¹⁶−10¹⁸ cm⁻²) and subsequent heat treatments in the temperature range 100–1000°C on the electrical properties and the spectrum of deep traps of undoped (concentration of electrons n = 1 × 10¹⁴−1 × 10¹⁶ cm⁻³), moderately Si-doped (n = (1.2−2) × 10¹⁷ cm⁻³), and heavily Si-doped (n = (2−3.5) × 10¹⁸ cm⁻³) epitaxial n-GaN layers grown on Al₂O₃ substrates by metal-organic chemical vapor deposition. It is found that, on electron irradiation, the resistivity of n-GaN increases, this is due to a shift of the Fermi level to the limiting position close to E _c −0.91 eV. The spectrum of deep traps is studied for the initial and electron-irradiated n-GaN. It is shown that the initial properties of the irradiated material are restored in the temperature range 100–1000°C, with the main stage of the annealing of radiation defects at about 400°C.     

Effects of Illumination on Ar<Superscript>+</Superscript>-Implanted <Emphasis Type="Italic">n</Emphasis>-Type 6H-SiC Epitaxial Layers

Argon ions were implanted into n-type 6H-SiC epitaxial layers at 600°C. Postimplantation annealing was carried out at 1,600°C for 5 min in an Ar ambient. Four implantation-induced defect levels were observed at E_C-0.28 eV, E_C-0.34 eV, E_C-0.46 eV, and E_C-0.62 eV by deep level transient spectroscopy. The defect center at E_C-0.28 eV is correlated with ED₁/ED₂ and with ID₅. The defect at E_C-0.46 eV with a capture cross section of 7.8 × 10⁻¹⁶ cm² is correlated with E1/E2, while the defect at E_C-0.62 eV with a capture cross section of 2.6 × 10⁻¹⁴ cm² is correlated with Z1/Z2. Photo deep level transient spectroscopy was also used to study these defects. Upon illumination, the amplitudes of the deep level transient spectroscopy (DLTS) peaks increased considerably. Two emission components of Z1/Z2 were revealed: one fast and the other slow. The fast component could only be observed with a narrow rate window. In addition, a new defect was observed on the low-temperature side of the defect at E_C-0.28 eV when the sample was illuminated. [rl](Received ...; accepted ...)