Structure and dielectric properties of Ba<Subscript>1−x</Subscript>Sr<Subscript>x</Subscript>ZnTi<Subscript>7</Subscript>O<Subscript>16</Subscript> hollandite ceramics

Hollandite-type Ba_1−xSr_xZnTi₇O₁₆ (x=0, 0.2, 0.4, 0.6, 0.8, and 1) ceramics have been synthesized by the conventional solid-state ceramic route. The phase purity and microstructure of these compositions have been characterized using x-ray diffraction (XRD) and scanning electron microscopy (SEM). The XRD analysis shows that an increase in strontium concentration in the A-site causes pairing of vacant tunnel sites, and hence the structure becomes unstable due to the collapse of the tunnel walls. The dielectric properties such as dielectric constant (ε_r), loss tangent (tan δ), and temperature variation of dielectric constant (τε_r) have been measured up to the 13 MHz region. The present study shows that zinc hollandites have relatively high dielectric constant and low loss tangent. The temperature variation of dielectric constant studies reveal that Ba-rich compositions have high positive τε_r and Sr-rich compositions have high negative τε_r in the 0–100°C region. Proper tailor making of these compositions has been attempted to arrive at near-zero temperature variation of the dielectric constant.     

Dielectric Properties and Microstructure of MgO-TiO<Subscript>2</Subscript>-ZnO-CaO Ceramics

The effects of CaTiO₃ addition on the microstructure, phase formation, and dielectric properties of MgO-TiO₂-ZnO ceramics were investigated. The sintering temperature of CaTiO₃-doped (Mg_0.63Zn_0.37)TiO₃ ceramics can be lowered to 1290°C when the additive is used. The dielectric properties are found to be strongly correlated with the amount of CaTiO₃ addition. At 1290°C, (Mg_0.63Zn_0.37)TiO₃ ceramic with 1.0 mol% CaTiO₃ exhibited a dielectric constant ε _r of 23.3, dielectric loss tan δ of 1 × 10⁻⁵, and temperature coefficient of capacitance (TCC) of 10 ppm/°C.     

Effects of annealing in O2 and N2 on the electrical properties of tantalum oxide thin films prepared by electron cyclotron resonance plasma enhanced chemical vapor deposition

The tantalum oxide thin films with a thickness of 14 nm were deposited at 95°C by electron cyclotron resonance plasma enhanced chemical vapor deposition (ECRPECVD), and annealed at various temperatures (700∼850°C) in O₂ and N₂ ambients. The microstructure and composition of the tantalum oxide thin films and the growth of interfacial silicon oxide layer were investigated and were related to the electrical characteristics of the film. Annealing in an O₂ ambient led to a high dielectric constant (ε_r(Ta₂O₅) = 24) as well as a small leakage current (E_bd = 2.3 MV/cm), which were due to the improved stoichiometry and the decreased impurity carbon content. Annealing in an N₂ ambient resulted in poor and nonuniform leakage current characteristics. The as-deposited tantalum oxide films were crystallized into δ-Ta₂O₅ after annealing at above 750°C regardless of the ambient. The leakage current of the film abruptly increased after annealing at 850°C probably because of the stress caused by thermal expansion or contraction.     

Experimental study of non-stoichiometry in Cd<Subscript>1−x</Subscript>Zn<Subscript>x</Subscript>Te<Subscript>1±δ</Subscript>

In this communication, the latest experimental results are presented on a composition of Cd_1−xZn_xTe_1±δ, both x and δ, determined by the high-precision, vapor-pressure scanning method. The space arrangement of the single-phase solidus volume of Cd_1−xZn_xTe_1±δ in the pressure-temperature-composition (P-T-X) phase space has been derived from direct vapor-pressure measurements in the temperature range up to 1,375 K. From the experimental data for x=0.0, 0.05, 0.1, 0.15, 0.25, 0.5, 0.75, 0.8, 0.9, and 1, the complete phase diagram of Cd_1−xZn_xTe_1±δ was constructed. Transformation of the diagram was traced for the whole range of existence of the Cd_1−xZn_xTe_1±δ solid solution as a function of ZnTe concentration. Increase of ZnTe in the solid solution results in the extension of the homogeneity range and a shift of the solidus toward Te, so that already for x≥0.15 the solidus does not contain the stoichiometric, (n_Cd+n_Zn):n_Te=50 mol.% plane. From detailed experimental studies, maximum non-stoichiometry as a function of the temperature was determined in a wide temperature range for Te and metal solubility. Temperature dependencies of the partial pressures of vapor-phase species for different crystal compositions, X_S=const, were deduced from the vapor-pressure experiment for the x=0.05 section of the diagram. From these results, relationships are derived between crystal composition, vapor pressure, and composition of the conjugated vapor.     

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).     

Experimental determination and thermodynamic calculation of the phase equilibria in the Cu-In-Sn system

The phase equilibria of the Cu-In-Sn system were investigated by means of the diffusion couple method, differential scanning calorimetry (DSC) and metallography. The isothermal sections at 110–900 C, as well as vertical sections at 10wt.%Cu–70wt.%Cu were determined. It was found that there are large solubilities of In in the ε(Cu₃Sn), δ(Cu₄₁Sn₁₁), and η phases in the Cu-Sn system, and large solubilities of Sn in the γ, η, and δ(Cu₇In₃) phases in the Cu-In system. The η phase was found to continuously form from the Cu-In side to the Cu-Sn side, and a ternary compound (Cu₂In₃Sn) was found to exist at 110 C. Thermodynamic assessment of the Cu-In-Sn system was also carried out based on experimental data of activity and phase equilibria using the CALPHAD method, in which the Gibbs energies of the liquid, fcc and bcc phases are described by the subregular solution model and that of compounds, including two ternary compounds, are represented by the sublattice model. The thermodynamic parameters for describing the phase equilibria were optimized, and agreement between the calculated and experimental results was obtained.     

Phase relations in Cu- RO1.5- O (R < Ho,Er, Yb) and gibbs energy of formation of Cu2R2O5 (R < Ho,Er, Yb) between 1000 and 1325K

Phase relations in Cu-RO_1.5-O(R < Ho,Er,Yb) ternary systems at 1273K have been established by isothermal equilibration of samples containing different ratios of Cu:R(R < Ho,Er,Yb) in flowing air or high purity argon atmosphere for four days. The samples were then rapidly cooled to ambient temperature and the coexisting phases were identified by powder x-ray diffraction analysis. Only one ternary oxide, Cu₂R₂O₅(R < Ho,Er,Yb) was found to be stable. The chemical potential of oxygen for the coexistence of the three phase assemblage, Cu₂O + R₂O₃ + Cu₂R₂O₅(R < Ho,Er,Yb) has been measured by employing the solid-state galvanic cells,< (−) Pt, Cu₂O + Ho₂O₃+ Cu₂Ho₂O₅//CSZ//Air (Po₂< 2.12 × 10⁴ Pa), Pt (+) (−) Pt, Cu₂O + Er₂O₃+ Cu₂Er₂O//CSZ//Air (Po₂< 2.12 × 10⁴ Pa), Pt (+) (−) Pt, Cu₂O + Yb₂O₃ + Cu₂Yb₂O₅//CSZ//Air (Po₂ < 2.12 × 10⁴ Pa), Pt (+) in the temperature range of 1000 to 1325K. Combining the measured emf of the above cells with the chemical potential of oxygen at the reference electrode, using the Nernst relationship, gives for the reactions, 2Cu₂O(s) + 2Ho₂O₃(s) + O₂(g) → 2Cu₂Ho₂O₅(s) (1) 2Cu₂O(s) + 2Er₂O₃(s) + O₂(g) → 2Cu₂Er₂O₅(s) (2) and 2Cu₂O(s) + 2Yb₂O₃(s) + O₂(g) → 2Cu₂Yb₂O₅(s) (3) δΜo₂ = −219,741.3 + 145.671 T (±100) Jmol⁻¹ (4) δΜo₂ = −222,959.8 + 147.98 T(±100) Jmol⁻¹ (5) and δΜo₂ = −231,225.2 + 151.847 T(±100) Jmol⁻¹ (6) respectively. Combining the chemical potential of oxygen for the coexistence of Cu₂O + R₂O₃ + Cu₂R₂O₅(R− Ho,Er,Yb) obtained in this study with the oxygen potential for Cu₂O + CuO equilibrium gives for the reactions, 2 CuO(s) + Ho₂O₃(s) → Cu₂Ho₂O₅(s) (7) 2 CuO(s) + Er₂O₃(s) → Cu₂Er₂O₅(s) (8) and 2 CuO(s) + Yb₂O₃(s) → Cu₂Yb₂O₅(s) (9) δG‡ < 22,870.3 − 23.160 T (±100) Jmol⁻¹ (10) δG‡ < 21,261.1 − 22.002 T (±100) Jmol⁻¹ (11) and δG‡ < 17,128.4 - 20.072 T (±100) Jmol^-1 (12) It can be clearly seen that the formation of Cu₂R₂O₅R < Ho,Er,Yb) from the component oxides is endothermic. Further, Cu₂R₂O₅(R < Ho,Er,Yb) are an entropy stabilized phases. Based on the results obtained in this study, the oxygen potential diagram for Cu-R-O(R < Ho,Er,Yb) ternary system at 1273K has been composed.     

An Extension of Kedlaya's Algorithm to Hyperelliptic Curves in Characteristic 2

We present an algorithm to compute the zeta function of an arbitrary hyperelliptic curve over a finite field F_q of characteristic 2, thereby extending the algorithm of Kedlaya for odd characteristic. Given a genus g hyperelliptic curve defined over F_qⁿ, the average-case time complexity is O(g^{4 + ε} n^{3 + ε}) and the average-case space complexity is O(g³ n³), whereas the worst-case time and space complexities are O(g^{5 + ε} n^{3 + ε}) and O(g⁴ n³), respectively.     

Microwave Dielectric Properties of ZnO-2TiO<Subscript>2</Subscript>-Nb<Subscript>2</Subscript>O<Subscript>5</Subscript> Ceramics with BaCu (B<Subscript>2</Subscript>O<Subscript>5</Subscript>) Addition

The influence of BaCu(B₂O₅) (BCB) addition on the sintering temperature and microwave dielectric properties of ZnO-2TiO₂-Nb₂O₅ (ZTN) ceramic has been investigated using dilatometry, x-ray diffraction, scanning electron microscopy, and microwave dielectric measurements. A small amount of BCB addition to ZTN can lower the sintering temperature from 1100°C to 900°C. The reduced sintering temperature was attributed to the formation of the BCB liquid phase. The ZTN ceramics containing 3.0 wt.% BCB sintered at 900°C for 2 h have good microwave dielectric properties of Q × f = 19,002 GHz (at 6.48 GHz), ε _r = 45.8 and τ _f  = 23.2 ppm/°C, which suggests that the ceramics can be applied in multilayer microwave devices, provided that Ag compatibility exists.     

Dielectric properties of FR-4 laminates as a function of thickness and the electrical frequency of the measurement

The relationship between the dielectric properties (dielectric constant, ε _lam ^′ and loss factor, ε _lam ^″ ) and thickness of FR-4 laminates was investigated. Thickness variations for laminates reinforced by the same style and number of plies of glass cloth were predominantly due to differences in the resin content. At each measurement frequency, values of both ε _lam ^′ and ε _lam ^″ were found to vary in an approximate linear manner with changes in the volume fraction of resin,V _rsn . An empirical equation was derived that gives the dielectric constant of an FR-4 laminate, ε _lam ^′ , as a function of the volume fraction of resin,V _rsn , and the frequency at which the measurement was performed (between 1 kHz and 1 GHz). An alternative expression was also determined that permits the calculation of ε _lam ^′ in the same frequency range from just the dielectric thickness of the laminate, providing the effective thickness of the reinforcement is known. The effective thickness of one style of glass cloth (2116) was experimentally determined to be 1.6 mils/ply. Effective thicknesses of most other common woven glass reinforcements used in FR-4 laminates were calculated and tabulated. The empirical relationships should be a valuable aid to electrical designers and others who need to know the frequency dependence of the dielectric properties of FR-4 laminates having different glass-to-resin ratios. Presented, in part, at the Fall 1988 Meeting of the IPC in Anaheim, California     

Mechanical fatigue of thin copper foil

The electrodeposited and the rolled 12 to 35 μm thick copper foils are subjected to the bending/unbending strain-controlled flex fatigue over a wide range of strain amplitudes. The fatigue life is associated with an increase in electrical resistance of the specimen beyond a preassigned threshold. For each foil type, in the rolled or as-deposited as well as in the (recrystallization-like) annealed conditions, the inverse Coffin-Manson (C-M) relationship between strain amplitude (Δε/2) and fatigue life (N_f) is established in the high Δε/2 (low N_f) and the low Δε/2 (high N_f) regimes. The N_f, Δε/2, and C-M slopes (c,b) are utilized to calculate the cyclic strain hardening (n′) and fatigue ductility (D_f) parameters. It is shown that for a given foil thickness, an universal relationship exists between D_f and the strength (σ) normalized fatigue life (N_f/σ). The propagation of fatigue crack through the foil thickness and across the sample width is related to the unique fine grain structure for each foil type: pancaked grains for the rolled foil and equiaxed grains for the electrodeposited foil. The fatal failure corresponds to convergence of the through-thickness and the across-the-width fatigue cracks. The variations in (i) electrical resistance, (ii) mid-thickness microhardness and grain structure and (iii) dislocation configurations with fatigue are monitored. Except for a small but significant fatigue induced softening (or hardening), no convincing evidence of strain localization (and the associated dislocation configurations generally observed for the bulk samples) has been found.     

Interfacial reactions in Ag-Sn/Cu couples

Interfacial reactions between Sn-3.5 wt.%Ag, Sn-25 wt.%Ag, and Sn-74 wt.%Ag alloys with Cu substrate at 240°C and 450°C have been studied here by examining the reaction couples. It is found that Sn is the fastest diffusion species among the three elements during the reaction, while Ag is the slowest. The reaction path is liquid/η/ɛ₁/Cu for the Sn-3.5 wt.%Ag/Cu couples reacted at 240°C. The paths are liquid/ɛ₁/δ/Cu, liquid/ɛ₁/δ/Cu, ɛ₂/ζ/ɛ₁/δ/Cu, for the Sn-3.5 wt.%Ag/Cu, Sn-25 wt.%Ag/Cu, and Sn-74 wt.%Ag/Cu couples at 450°C, respectively. These reaction paths are in agreement with the isothermal sections of the Ag-Sn-Cu ternary system at 240°C and 450°C. The isothermal sections are proposed based on the limited ternary phase equilibria data and the phase diagrams of its three constituent binary systems, Ag-Sn, Cu-Sn, and Ag-Cu.     

Self-Diffusion in gallium arsenide

The self-diffusion of arsenic in gallium arsenide has been studied over the temperature range 1000 to 1075δC using radiotracer techniques.⁷⁶As was diffused into GaAs samples at known arsenic pressures in sealed capsules. After diffusion, layers were removed from the surface using anodic oxidation followed by oxide dissolution. Diffusion profiles were obtained by measuring the⁷⁶As concentration in each sectioned layer by γ-radiation counting. Diffusion coefficients at P_{As 2} = 0.75 atm and over the temperature range 1000 to 1050δC were found to be 5.2 × 10^-16cm²s^-1 to 1.5 × 10^-15 cm²s^-1, leading to an activation energy of the order of 3.0^± 0.04 eV and a pre-exponential factor of 5.5 × l0^-4 ± 2.4 × 10^-4 cm²s^-1. Diffusion coefficients at P_{As 2} =3.0 atm were found to be 5.5 × 10^-15 and 9.8 × 10^-16 cm² s^-1 at 1050 and 1075δC, respectively. Results are discussed in terms of native point defect equilibria with the arsenic gaseous phase, and with respect to other work. It is deduced from our observed arsenic pressure dependence of the arsenic diffusivity that the most likely diffusion mechanism     

Growth of intermetallic compounds in the Sn-9Zn/Cu joint

We have studied the microstructure of the Sn-9Zn/Cu joint in soldering at temperatures ranging from 230°C to 270°C to understand the growth of the mechanism of intermetallic compound (IMC) formation. At the interface between the Sn-9Zn solder and Cu, the results show a scallop-type ε-CuZn₄ and a layer-type γ-Cu₅Zn₈, which grow at the interface between the Sn-9Zn solder and Cu. The activation energy of scallop-type ε-CuZn₄ is 31 kJ/mol, and the growth is controlled by ripening. The activation energy of layer-type γ-Cu₅Zn₈ is 26 kJ/mol, and the growth is controlled by the diffusion of Cu and Zn. Furthermore, in the molten Sn-9Zn solder, the results show η-CuZn grains formed in the molten Sn-9Zn solder at 230°C. When the soldering temperature increases to 250°C and 270°C, the phase of IMCs is ε-CuZn₄.     

Permittivity and Conductivity Measurements of Building Materials at 5.8 GHz and 41.5 GHz

The results of various experiments performed to characterize electromagnetic properties of typical building materials at BRAN (Broadband Radio Access Networks) and MVDS (Multipoint Video Distribution System) bands are presented and compared. Transmission and reflection coefficients were measured as functions of the angle of incidence, using a wideband sounder based on the swept frequency technique. A high precision angular positioning system was built and used in co-ordination with the measurement equipment.The dielectric constants (_r) were estimated by comparing values predicted with a multiple successive internal reflection model and measured transmission and reflection coefficients. It has been found that the variation of the dielectric constant value with the frequency does not necessarily follow the same trend for different materials. For example, the measured _r for plasterboard presents an increment withfrequency (2.02 at 5.8 GHz, 2.5 at 41.5 GHz – measured by theauthors –, 2.58 at 59.5 GHz, and 2.81 at 60.2 GHz – given byliterature –), while the values for glass follow a wanderingpattern (6.06 at 5.8 GHz, 5–10 at 10 GHz, 3.41 at 41.5 GHz, 7.51at 57.6 GHz, and 5.29 at 60.2 GHz). Moreover, the measured_r for a brick wall at 5.8 GHz (3.58) shows differenceswith values reported at 2 GHz (4.44).     

Phase Transitions in the BiVO<Subscript>4</Subscript>-<Emphasis Type="Italic">n</Emphasis>PbO (<Emphasis Type="Italic">n</Emphasis> = 1, 2) System: Structural–Electrical Properties Relationships

In a general survey of nPbO-BiVO₄ compounds, interesting phases corresponding to n = 1: PbBiVO₅, and n = 2: Pb₂BiVO₆ are described. A phase transition has been unambiguously characterized for PbBiVO₅. The crystal structures were solved from twinned crystals at room temperature (α phase, triclinic, S.G. P-1) and at 530°C (β phase, monoclinic, C2/m). Powder neutron diffraction experiments confirmed these settings and both room-temperature (RT) and high-temperature (HT) refinements corroborated space group choices, clearing up a literature controversy about the centrosymmetry of the α phase, and identifying structural modifications occurring under the α → β transition. Cationic substitutions for V were tested and PbBi(V_1−x M _x )O₅ (M = P) solid solutions identified. Pb₂BiVO₆ (n = 2) is a compound showing several successive structural transitions, i.e., α → β → δ. Structures of α and δ forms have been previously described from powder diffraction data (x-ray and neutron). In this work, we have refined these structures from single-crystal data, and the resolution of the intermediate β form, so far unsolved, was possible through a stabilization thermal cycle; its complete structural understanding required a 4D formalism. Two new polymorphic phases, α′ and δ′, were obtained by substituting Mn or P for V; their structures are closely related to, respectively, the α phase at room temperature, and the δ phase at 680°C. Electrical conductivities of all structurally characterized compositions were investigated, and correlations were drawn between their conduction properties and structural characteristics. Conductivity properties measured under variable O₂ partial pressures for Pb₂Bi(V_0.75P_0.25)O₆ were interpreted as a mixed ionic–electronic (p-type) conduction mechanism.     

Orientation texture in YBa2Cu3O7−δ films synthesized from amorphous precursors

The metalorganic decomposition technique was utilized in the fabrication of YBa₂Cu₃O_7−δ films with preferred orientation on (100) MgO and (100) SrTiO₃ substrates. The processing parameters such as film thickness, firing treatment, and substrate modifications were controlled to obtain a high degree of three-dimensional preferred growth in the films. Results indicate that three-dimensional film preferred growth diminishes with increasing film thickness. Preferential growth in YBa₂Cu₃O_7−δ films is enhanced with increasing firing temperature and reduced oxygen partial pressure due to enhanced atom mobility. Epitaxial growth of YBa₂Cu₃O_7−δ films has been achieved on both lattice mismatched (MgO) and on lattice matched (SrTiO₃) substrates. Epitaxial growth is promoted by lattice matched substrates at lower film firing temperatures. An attempt is made to understand the development of YBa₂Cu₃O_7−δ film preferential growth via the epitaxial grain growth mechanism.     

Overview of fatigue performance of Cu processed by severe plastic deformation

This study investigates discrepancies regarding cyclic softening of Cu processed by severe plastic deformation (SPD). All samples softened if the microhardnesses before and after fatiguing are compared. However, the effect decreases if the strain amplitude is small, Δε_p <1 × 10⁻³). Samples with equiaxed subgrains were more resistant to softening and thermal recovery. All samples had “persistent” shear bands except those tested at the highest amplitudes, Δε_p >1 × 10⁻². Cu processed by SPD exhibits an enhanced fatigue life at low amplitudes. However, low thermal stability, potential for softening, and poor low-cycle properties discredit this advantage.     

Interfacial Reactions of Sn-8wt.%Zn-3wt.%Bi Solder with Cu,Ag, and Ni Substrates

Sn-Zn-Bi alloys are promising Pb-free solders. Interfacial reactions between the Sn-8wt.%Zn-3wt.%Bi (Sn-13.80at.%Zn-1.62at.%Bi) alloy and the Cu, Ag, and Ni substrates are examined. Two different kinds of substrates, the bulk plate and the electroplating layer, are used, and the reactions are carried out at 250°C and 220°C. Although the Zn content is only 13.8 at.%, two Zn-Cu compounds, γ-Cu₅Zn₈ and ε-CuZn₅ phases, are formed in the Sn-13.80at.%Zn-1.62at.%Bi/Cu couples. The ε-CuZn₅ phase is scallop shaped, and the γ-Cu₅Zn₈ phase is planar. In the Sn-13.80at.%Zn-1.62at.%Bi/Ag couples, three Zn-Ag compounds are observed, and they are ε-AgZn₃, γ-Ag₅Zn₈, and ζ-AgZn phases. In the Sn-13.80at.%Zn-1.62at.%Bi/Ni couples, a Zn-Ni compound, γ-Ni₅Zn₂₁ phase, is formed. Similar results are found in the couples prepared with an electroplating layer: the reaction phases are the same, but the growth rates are different.     

Intermetallic reactions in Sn-8Zn-20In solder ball grid array packages with Au/Ni/Cu and Ag/Cu pads

During the reflow process of Sn-8Zn-20In solder joints in the ball grid array (BGA) packages with Au/Ni/Cu and Ag/Cu pads, the Au and Ag thin films react with liquid solder to form γ₃-AuZn₄/γ-Au₇Zn₁₈ and ε-AgZn₆ intermetallics, respectively. The γ₃/γ intermetallic layer is prone to floating away from the solder/Ni interface, and the appearance of any interfacial intermetallics cannot be observed in the Au/Ni surface finished Sn-8Zn-20In packages during further aging treatments at 75°C and 115°C. In contrast, ε-CuZn₅/γ-Cu₅Zn₈ intermetallics are formed at the aged Sn-8Zn-20In/Cu interface of the immersion Ag BGA packages. Bonding strengths of 3.8N and 4.0N are found in the reflowed Sn-8Zn-20In solder joints with Au/Ni/Cu and Ag/Cu pads, respectively. Aging at 75°C and 115°C gives slight increases of ball shear strength for both cases.