Zili Kou

Ultrahigh-pressure densification of nanocrystalline WB ceramics

Phase-pure nanostructured WB ceramics are hot pressed at ultrahigh pressures of 1.0 to 3.0 GPa and high temperatures of 700 to 1000 °C (UHPHT) for 60 min. The UHPHT samples are nanograin size from 15 to 40 nm. Our experimental observation shows that ultrahigh pressure could improve densification, and the density of WB samples could reach 99.4% of theoretical. The comparative experiments carried out at ambient pressure and temperatures of 550 to 1100 °C for 60 min indicate that the external pressure was favorable for phase-pure and highly dense WB formation. In addition, the UHPHT samples give a high hardness value of 28.9 ± 0.8 GPa.

Diamond-cBN alloy: A universal cutting material

Diamond and cubic boron nitride (cBN) as conventional superhard materials have found widespread industrial applications, but both have inherent limitations. Diamond is not suitable for high-speed cutting of ferrous materials due to its poor chemical inertness, while cBN is only about half as hard as diamond. Because of their affinity in structural lattices and covalent bonding character, diamond and cBN could form alloys that can potentially fill the performance gap. However, the idea has never been demonstrated because samples obtained in the previous studies were too small to be tested for their practical performance. Here, we report the synthesis and characterization of transparent bulk diamond-cBN alloy compacts whose diameters (3 mm) are sufficiently large for them to be processed into cutting tools. The testing results show that the diamond-cBN alloy has superior chemical inertness over polycrystalline diamond and higher hardness than single crystal cBN. High-speed cutting tests on hardened steel and granite suggest that diamond-cBN alloy is indeed a universal cutting material

Note: An anvil-preformed gasket system to extend the pressure range for large volume cubic presses

An anvil-preformed gasket system has been developed to extend the pressure range for the widely used large volume cubic press without sacrificing the sample volume. The relationship of the sample chamber pressure versus press load for this system was calibrated at room temperature using transitions in Bi, Tl, and Ba. With similar sample volumes (8-11 mm in diameter and 8 mm in length), the anvil-preformed gasket system can generate pressures up to about 8.5 GPa, significantly higher than 6 GPa, which was generally the maximum pressure for the conventional anvil-gasket system. The details on the optimized design for the anvil-preformed gasket system are given in this note.

Submicron cubic boron nitride as hard as diamond

Here, we report the sintering of aggregated submicron cubic boron nitride (sm-cBN) at a pressure of 8 GPa. The sintered cBN compacts exhibit hardness values comparable to that of single crystal diamond, fracture toughness about 5-fold that of cBN single crystal, in combination with a high oxidization temperature. Thus, another way has been demonstrated to improve the mechanical properties of cBN besides reducing the grain size to nano scale. In contrast to other ultrahard compacts with similar hardness, the sm-cBN aggregates are better placed for potential industrial application, as their relative low pressure manufacturing perhaps be easier and cheaper.

High pressure and high temperature sintering of fine-grained PCD using bi-layered assembly

This work presents the study of the synthesis and characterization of polycrystalline diamond (PCD) compacts using a bi-layered assembly method and solving the catastrophic nature of failure molding when using single-layered assembly and 0.5–1.5 μm diamond powder as starting materials. The well-sintered PCD compacts are prepared on WC-16wt% Co substrates at temperatures from 1350 °C to 1500 °C for 15 min at static high pressure of 5.2 GPa, using the bi-layered assembly method. According to our scanning electron microscope observation, the specimens sintered at 1450 °C have a homogeneous microstructure. The graphitization of the diamond appears at 1500 °C according to X-ray diffraction analysis. The specimens sintered at 1450 °C show the best performance according to the wear resistance test.

High pressure sintering behavior and mechanical properties of cBN–Ti3Al and cBN–Ti3Al-Al composite materials

The sintering behavior and mechanical properties of cubic boron nitride (cBN) composites, using the mixture of cBN–Ti3Al and cBN–Ti3Al-Al as the starting material respectively, were investigated under high pressure and high temperature (HPHT) conditions. The results show that the samples of cBN–Ti3Al-Al sintering system have more homogeneous microstructures. Youngs modulus, shear modulus, and bulk modulus of samples measured by ultrasonic measurements can reach to 782±3 GPa, 344±1 GPa, and 348±2 GPa, respectively. The hardness increases remarkably with the sintering temperature rising, and reaches to the highest value of 35.04±0.51 GPa. For the cBN–Ti3Al sintering system, the X-ray diffraction patterns of composites reveal that the chemical reactions between cBN and Ti3Al occurred at 5.0 GPa and 1300°C. The reaction mechanisms of both cBN–Ti3Al and cBN–Ti3Al-Al sintering systems are discussed in this paper.

High pressure sintering behavior of polycrystalline diamond with tungsten

Polycrystalline diamond was investigated under high pressure and high temperature of 5.0 GPa and 1100–1500 °C in the presence of tungsten. In situ resistance measurements indicated that reactions between diamond and tungsten happened at about 960 °C. Phase analysis demonstrated that WC increased and meta-stability of W2C decreased clearly at the higher temperature. It is clear from the characterization of the sintered body that the electrical resistance decreased and the density of specimens increased as the sintering temperature rose. The specimen sintered at 1500 °C has a homogeneous microstructure and good conductivity.

Neutron powder diffraction and high-pressure synchrotron x-ray diffraction study of tantalum nitrides*

Tantalum nitride (TaN) compact with a Vickers hardness of 26 GPa is prepared by a high-pressure and hightemperature (HPHT) method. The crystal structure and atom occupations of WC-type TaN have been investigated by neutron powder diffraction, and the compressibility of WC-type TaN has been investigated by using in-situ high-pressure synchrotron x-ray diffraction. The third-order Birch–Murnaghan equation of state fitted to the x-ray diffraction pressure–volume (P – V) sets of data, collected up to 41 GPa, yields ambient pressure isothermal bulk moduli of B 0 = 369(2) GPa with pressure derivatives of for the WC-type TaN. The bulk modulus of WC-type TaN is not in good agreement with the previous result (B 0 = 351 GPa), which is close to the recent theoretical calculation result (B 0 = 378 GPa). An analysis of the experiment results shows that crystal structure of WC-type TaN can be viewed as alternate stacking of Ta and N layers along the c direction, and the covalent Ta–N bonds between Ta and N layers along the c axis in the crystal structure play an important role in the incompressibility and hardness of WC-type TaN.

Superstrong micro-grained polycrystalline diamond compact through work hardening under high pressure

We report an approach to strengthen micro-grained polycrystalline diamond (MPD) compact through work hardening under high pressure and high temperature, in which both hardness and fracture toughness are simultaneously boosted. Micro-sized diamond powders are treated without any additives under a high pressure of 14 GPa and temperatures ranging from 1000 °C to 2000 °C. It was found that the high pressure and high temperature environments could constrain the brittle feature and cause a severe plastic deformation of starting diamond grains to form a mutual bonded diamond network. The relative density is increased with temperature to nearly fully dense at 1600 °C. The Vickers hardness of the well-prepared MPD bulks at 14 GPa and 1900 °C reaches the top limit of the single crystal diamond of 120 GPa, and the near-metallic fracture toughness of the sample is as high as 18.7 MPa m1/2.

Preparation of superhard cubic boron nitride sintered from commercially available submicron powders

Using submicron cubic boron nitride (cBN) powder as a starting material, polycrystalline cBN (PcBN) samples without additives were sintered from 8.0–14.0 GPa at 1750 °C, and their sintering behaviour and mechanical properties were investigated. Transmission electron microscopy analysis showed that high-density nanotwins could be generated from common submicron cBN grains during high pressure and high temperature treatment. The dislocation glide and (111) mechanical micro-twinning are the main mechanisms that underlie plastic deformation in the sintering process, and this contributes to the grain refinement. A refinement in the grain size (∼120 nm), micro-defect (nanotwin and stacking faults), and strong covalent bonding between the grains are crucial for improving the sample mechanical properties. The PcBN sintered at 11.0 GPa/1750 °C possessed outstanding mechanical properties, including a high Vickers hardness (∼72 GPa), fracture toughness (∼12.4 MPam1/2), and thermal stability (∼1273 °C in air).