Compositions,mechanical properties and microstructures of cBN-based composites sintered with Al or TiC

Cubic boron nitride (cBN)-based composites were prepared from cBN–Al and cBN–TiC mixtures, respectively, under high pressure and high temperature (HPHT). During sintering, Al reacted with cBN and produced AlN and AlB₂, while TiC did not react with cBN. With increasing Al from 5–20?wt-%, the strength of the cBN-based composites decreased first, then increased. AlN and AlB₂ could strengthen the cBN-based composites to a certain extent. In the preparation from cBN–TiC, 10?wt-% addition of TiC was the optimal formulation to obtain the densest microstructure. Hardness of the two kinds of composites displayed different tendencies. On the other hand, cBN-based composites were treated at 1200°C for 1200?s. It was found that the isothermal oxidation process could be described by parabolic laws with slight oxidation scales formed on samples’ surfaces in different morphologies.     

Effects of trimethylamine and ammonia on cBN content in the samples prepared by hydrothermal method

The previous results have proved that the phase-selective synthesis route is an effective method for preparing cubic boron nitride (cBN) from hydrothermal solutions. However, the experimental parameters are still required to be optimized in order to synthesize pure cBN at high yield. Here we report the results of investigating the effects of adding trimethylamine (N(CH₃)₃) and ammonia (NH₃·H₂O) (denoted as secondary nitrogen source) into the reacting solutions. It was found that the content of cBN could be increased by adding appropriate amount of N(CH₃)₃ and decreased with excess amount of it. On the contrary, hexagonal boron nitride (hBN) was always promoted by adding NH₃·H₂O into the reacting solutions. The samples were characterized by X-ray powder diffraction (XRD), Fourier transform infrared spectrum (FTIR) and high resolution transmission electron microscopy (HRTEM). The experimental results were briefly discussed based on a reported model.     

On the low-temperature threshold for cubic boron nitride formation in energetic film deposition

The sharp threshold in substrate temperature below which cubic boron nitride (cBN) cannot be formed in energetic film-deposition processes was investigated. We found that cBN could be synthesized below the threshold temperature on top of cBN that had been previously formed above the threshold temperature. That the initial nucleation of cBN is more strongly dependent on temperature than its subsequent growth is suggested. How the structure of the sp²-bonded BN that accompanied cBN growth changed with temperature was also investigated. Lowering the substrate temperature decreased the local ordering within the graphitic planes, and below the threshold temperature the separation of the graphitic planes increased dramatically. How these structural changes may influence the nucleation of cBN is discussed.     

Defect-induced electronic conduction of tBN thin films

Two kinds of turbostratic boron nitride (tBN) thin films were deposited by sputtering with pure Ar or N₂ plasma in an ultraclean vacuum chamber. Current–voltage (I–V) characteristics of Ti/tBN/Ti structures revealed that films deposited in Ar showed at least three-orders higher conductivity with strong temperature and electric field dependence compared with those deposited in pure N₂. The origin of the higher conductivity was confirmed to be the nonstoichiometry and higher defect density of the tBN films. On the other hand, films deposited in pure N₂ plasma showed the characteristics of intrinsic insulator even though the basal plane of tBN was oriented normal to the substrate, namely, parallel to the direction of electronic conduction.     

Tool wear characteristics analysis of cBN cutting tools in high-speed turning of Inconel 718

Nickel-based superalloy is a critical material for turbine engine components in the aerospace application, but the poor machinability and low machining efficiency have further hampered it to be used widely. Cubic boron nitride (cBN), having extreme hardness and chemical inertness, is the potential candidate to process superalloys. In this paper, we systematically investigated the tool wear characteristic of cBN at different cutting speeds in dry turning of Inconel 718 by experiments and FEM simulations. The FEM model with initial flank wear land (VB) was established and validated. Effects of cutting speeds (200–400 m/min) on cBN tool life and wear mechanisms were systematically investigated. Effects of tool flank wear on cBN tool cutting edge temperature field and Inconel 718 machined surface layer stress distribution were analyzed by FEM simulations.     

In-situ X-ray observation of phase transformation of rhombohedral boron nitride under static high pressure and high temperature

In-situ X-ray diffraction study for phase transformation of rhombohedral boron nitride (rBN) to a denser phase was performed under static high pressure (HP) and high temperature (HT) up to 9 GPa and 1600 °C. It was found that the layer stacking sequence of rBN structure began to change at less than 1 GPa, and the phase transformation to wurtzite structure (wBN) was observed at 6–7 GPa and room temperature. After conversion to wBN, further transformation to the zincblend type cubic structure (cubic BN) at 8 GPa and 1400 °C was observed, which is quenchable and the P-T conditions yielding cBN form were similar to that from hexagonal boron nitride. The observed behavior of the phase transformation of rBN by using in-situ X-ray diffraction study is well consistent with the results obtained from the quenching experiment from HP/HT by using belt type HP apparatus.

No structural change was observed at 600°C isothermal compression up t0 8GPa, while wBN formation was observed at room temperature compression at 7 GPa. This variation of the transformation behavior under HT isothermal compression may essentially be caused by the reduction of shear stress which affects the rotation and/or slip of hexagonal plane of rBN under HP.     

First Principles Study of the Aluminum-Cubic Boron Nitride Interface

A plane wave density functional methodology, with the local density approximation for the elemental constituents, was used to investigate the structure, bonding, and adhesion of atomic-scale interfaces between aluminum and cubic-boron nitride (c-BN). Two fully periodic interfaces, Al(110)-c-BN(110) and Al(001)-c-BN(110), were constructed for this purpose. Interfacial bonding, examined with contours of the charge density difference and electron localization function, was found to be stronger between Al-N pairs than Al-B pairs. The computed work of separation ( W_s ) values were 2.25 J/m² for Al(110)-c-BN(110) and 2.65 J/m² for Al(001)-c-BN(110). The higher adhesion in the latter interface is attributed to a higher planar density of interfacial Al atoms. The computed W_s values were compared with values from first principles calculations on other aluminum-ceramic interfaces. The possibility of adhesive transfer during tensile debonding was qualitatively investigated.     

The effect of boron nitride nanosheets on the mechanical and thermal properties of aluminum nitride ceramics

The boron nitride nanosheets (BNNSs)/aluminum nitride (AlN) composites were prepared by hot press sintering at 1600°C. The microstructure, mechanical properties, and thermal conductivity of the samples were measured, and the effect of adding BNNSs to AlN ceramics on the properties was studied. It is found that the addition of BNNSs can effectively improve the mechanical properties of AlN. When the additional amount is 1 wt%, the bending strength of the sample reaches the maximum value of 456.6 MPa, which is 23.1% higher than that of the AlN sample without BNNSs. The fracture toughness of the sample is 4.47 MPa m^1/2, a 68.7% improvement over the sample without BNNSs. The composites obtained in the experiment have brilliant mechanical properties.     

CBN grain wear during eco-benign grinding of nickel-based superalloy with oscillating heat pipe abrasive wheel

Cubic boron nitride (CBN) has high hardness and superior thermal conductivity, and it was used to fabricate an oscillating heat pipe abrasive wheel (OHPGW) for the eco-benign grinding of hard-to-machine materials. Furthermore, the wear behavior of the CBN grains and the related lifecycle of the OHPGW are important. In this study, a comparative analysis was conducted to reveal the wear behavior of CBN grains on OHPGWs and conventional wheels. Under the enhanced heat transfer effect of the OHPGW, the CBN grain wear behavior, development of the CBN protrusion heights, and the ground surface quality were investigated. The CBN grains on the abrasive wheel experience initial, stable, and fast wear periods in conditions of attrition, micro-fracture, and macro-fracture. Owing to the low grinding heat and temperature acting on the OHPGW, the CBN grains mostly undergo attrition during the stable period, while CBN grains on the conventional wheel mainly undergo micro and macro-fractures. As the wear of the CBN grains progressed, the average protrusion height of the CBN grains decreased. The scattering of the protrusion height distribution decreased at first and then increased when entering the fast wear period. Consequently, the surface topography and roughness initially improved and then deteriorated with the development of the protrusion height distribution of the CBN grains.     

Application of h-BN particles using Ca-assisted carbothermal reduction nitridation to high-thermal-conductive resin/h-BN composites

Hexagonal boron nitride (h-BN) particles exhibit high thermal conductivity and are promising fillers for resin filling. However, h-BN particles are plate-like particles with thermal anisotropy in the planar and thickness directions. Therefore, their applications are limited due to low thermal conductivity in the direction of the thickness of a resin sheet filled with h-BN particles. In this study, we control the size and thickness of h-BN particles using carbothermal reduction nitridation (CRN), which involves the carbothermic reduction of boric oxide in an N₂ gas atmosphere and develop them into resin sheets. In CRN using a CaO promoter, a novel method is developed to control the shape, size, and thickness of h-BN particles. Using h-BN particles grown in the thickness direction, we have successfully provided resin sheets with high thermal conductivity.     

The wetting-to-nonwetting transition of CVD BN coatings deposited at different temperatures

Boron nitride (BN) coatings (thickness 20–40 μm) were prepared on graphite substrates by chemical vapor deposition, with precursors of BCl₃ and NH₃ (ratio of 1:4) and pressure of 500 ± 50 Pa. The influence of the deposition temperature (650°C–1250°C) on the wettability of BN coatings with deionized water was studied. The wetting angle rapidly increases at 1100°C–1250°C, and the wetting-to-nonwetting transition occurs. The crystal structure and surface morphology of the BN coatings were characterized by a stylus instrument, scanning electron microscopy, and transmission electron microscopy. Research shows that the contact angle or nonwettability increases with a higher degree of crystallinity and a lower surface roughness, which were both under the control of the deposition temperature since the pressure and gas flows were kept constant in this study. At a deposition temperature of 650°C–950°C, the increase in the degree of crystallinity dominates; at 950°C–1100°C, the increase in surface roughness takes over. At 1100°C–1250°C, the degree of crystallinity continues to increase, while the surface roughness decreases due to the advantage of nucleation and the breakage of large surface clusters into smaller clusters. This results in increases (650°C–950°C), then decreases (950°C–1100°C) and again fast increases (1100°C–1250°C) in the wetting angle between the BN coating and deionized water and finally in the wetting-to-nonwetting transition (1100°C–1250°C).     

Recrystallization behaviour of cubic boron nitride under high pressure

The recrystallization behaviour of micron-sized cubic boron nitride (cBN) was studied by analysing the grain size and morphology of samples treated at 8−16 GPa/1500–2200 °C. The results show that the recrystallization temperature of cBN under a pressure of 8 GPa is approximately 1650 °C and increases by approximately 100 °C with every 2 GPa increase in pressure. Once grain recrystallization starts, the grains grow abnormally quickly as the temperature rises, and the strengthening effects of grain refinement and defect structure are greatly weakened. The recrystallization behaviour of cBN at high pressure is helpful to understand the sintering mechanism and control the microstructure and mechanical properties of sintered polycrystalline cBN compacts. In addition, the melting curve for cBN under high pressure is inferred according to the empirical relationship between recrystallization temperature and melting temperature, and the phase diagram for boron nitride is revised based on this new melting curve.     

Deposition of cubic boron nitride films on diamond-coated WC:Co inserts

Cubic boron nitride (cBN) thin films were deposited on diamond-coated tungsten carbide (WC) cutting inserts using electron cyclotron resonance (ECR) microwave plasma chemical vapor deposition (MPCVD). The effects of gas flow rate and substrate bias on the phase composition and structure of the BN films deposited on diamond surfaces were studied. It was revealed that both the cubic phase formation and the selective etching of hexagonal phase were controlled by modulating the hydrogen and boron trifluoride flow rate ratio. By the trial and error method the gas flow rate ratio and substrate bias voltage were optimized. Moreover the phase composition of the BN film was found to be affected by the thickness of diamond buffer layer and interrelated to the effective substrate bias. The hardness of the resulting cBN films reached the value of 70 GPa. In the synthesized coatings, the diamond beneath renders the best mechanical supporting capacity while the top cBN provides the superior chemical resistance and extreme hardness. The cBN/diamond bilayers deposited on WC inserts may serve as universal tool coatings for machining steels and other ferrous metals.     

差热分析在硅酸盐工业中的应用

论述了差热分析技术在硅酸盐工业中的应用,着重讨论了利用差热分析技术研究硅酸盐工业原材料的优选及单节技术方面等问题。     

Noncovalent functionalization of boron nitride and its effect on the thermal conductivity of polycarbonate composites

Polycarbonate (PC) is an engineering thermoplastic with excellent insulation and mechanical properties. However, the low thermal conductivity restricted its application in electronic devices. Hexagonal boron nitride (h ‐BN) microparticle, a promising material with high thermal conductivity, was functionalized with cationic polyacrylamide (CPAM) and introduced into PC matrix to improve the thermal conductivity. SEM and XRD analysis showed that the modified BN (CBN) particles oriented and formed thermal conductive pathways within PC matrix. The formation of large‐area oriented CBN significantly improved the thermal conductivity and thermal stability of composites. At 20 wt % CBN loading, the thermal conductivity of 0.7341 Wm^?1 K^?1 and the temperature for 5% weight loss (T ₅) of 498.6 °C were obtained, which was 3.1 times and 77 °C higher than that of pure PC, respectively. Furthermore, outstanding electrical insulation property of matrix was retained in the composites. These results revealed that PC/CBN composite was a promising material for thermal management and electrical enclosure. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134 , 44978.     

Bilayered coatings of BN/diamond grown on Si3N4 ceramic substrates

Cubic boron nitride (c-BN) is a well known material to be used in machining of ferrous metallic alloys, namely as a coating. However, in most practical cases, there is a lack of adhesion to the substrate material. In this work, BN coatings were deposited by magnetron sputtering on silicon nitride (Si₃N₄) ceramic substrates using an intermediate layer of CVD microcrystalline (MCD) or nanocrystalline diamond (NCD). The goal was to improve the c-BN content by using diamond interlayers, and to optimize film adhesion to the substrate by employing such ceramic, which is known to provide very high adhesion strength to CVD diamond. The BN/NCD/Si₃N₄ combination demonstrated to be unique regarding the absence of delamination at both the BN/diamond and diamond/substrate interfaces, also providing the highest c-BN phase content.     

Growth of cubic boron nitride films by ibad and triode sputtering: development of intrinsic stress

Two methods are employed to evidenced the stress behavior in c-BN films. On the one hand, in depth stress profile of c-BN film, deposited by ion beam assisted evaporation, was performed by recording infrared spectra and substrate curvature after reactive ion etching (RIE) steps. It shows a peak of stress up to −17 GPa in the h-BN basal layer and a stress relaxation when the cubic phase appears. On the other hand, dynamic stress profiles of c-BN films deposited by a triode sputtering system, are obtained by recording infrared spectra and substrate curvature after various c-BN deposition times, with the same experimental conditions. Likewise, a peak of stress of −12 GPa is unmistakably observed in the h-BN basal layer followed by a stress release during c-BN nucleation, where an average value of −12 GPa is observed in the c-BN film volume. These results provide a support for the stress model proposed by McKenzie even if along with a minimum stress a high level of densification of the layer is needed.     

氮化硼表面修饰及其对氮化硼/硅橡胶复合材料热性能的影响

研究氮化硼表面改性及其对氮化硼/硅橡胶复合材料热性能的影响。结果表明:活化可以提高氮化硼表面接枝率,偶联剂CA1对氮化硼的改性效果优于偶联剂KH570;随着氮化硼用量的增大,氮化硼/硅橡胶复合材料的热导率增大;加入氮化硼的复合材料热稳定性提高,但改性氮化硼/硅橡胶复合材料的热稳定性下降。     

Kinetic study of the II-I phase transition of isotactic polybutene-1

Kinetics of the solid-solid II-I phase transition of isotactic polybutene-1 was investigated. The fraction W_I of phase I as a function of time t_tr during the phase transition was measured by X-ray diffraction at various temperatures T_tr. The Avrami indices n of the W_I-t_tr plots are approximately unity for T_tr > 288 K. A bell-shaped temperature dependence of the transition rate V with the maximum transition rate at 285 K was obtained. The V-T_tr curve and the Avrami index n = 1 suggest that the rate-determining process is primary nucleation. The dependence of V on T_tr for T_tr < 283 K is described by the William-Landel-Ferry (WLF) equation, which shows that the glass transition affects the transition rate. The Avrami index decreases to n < 1 for T_tr < 283 K, indicating a broadened distribution of the transition rate caused by the spatial heterogeneity of the amorphous state at low temperatures near the glass transition. Those evidences at low temperature clearly suggest that the solid-solid phase transition is influenced by the mobility of chain folding, tie chains and cilia in the amorphous between the stacks of lamellar crystals.     

BN基复合陶瓷致密化的主要障碍

本文对ＢＮ基复合陶瓷进行了热压和无压烧结试验,对烧结体的密度变化和显微结构进行了研究,分析了影响ＢＮ基复合致密化的主要因素,认为卡片房式结构是妨ＢＮ基复合陶瓷致密化的主要原因。热压过程中施加的压力足够大时,可以破坏这种卡片房式结构,使片状ＢＮ定向排列,因而能获得同致密度的ＢＮ基复合陶瓷,热压过程中若有液相出现,有利于片状ＢＮ定向排列,因而能促进ＢＮ基复合陶瓷的致密化。无压烧结因不能消除坯体中的卡片