Synthesis and characterisation of Φ62 mm polycrystalline diamond compact

Journal Pre-proof Synthesis and characterisation of Φ62 mm polycrystalline diamond compact

Xuefeng Yang, Fuming Deng PII:

S0925-9635(19)30415-7

DOI:

https://doi.org/10.1016/j.diamond.2019.107594

Reference:

DIAMAT 107594

To appear in:

Diamond & Related Materials

Received date:

24 June 2019

Revised date:

16 October 2019

Accepted date:

21 October 2019

Please cite this article as: X. Yang and F. Deng, Synthesis and characterisation of Φ62 mm polycrystalline diamond compact, Diamond & Related Materials (2019), https://doi.org/ 10.1016/j.diamond.2019.107594

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© 2019 Published by Elsevier.

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Synthesis and Characterisation of Φ62 mm Polycrystalline Diamond Compact Xuefeng Yang*，Fuming Deng**1

Institute of Super-hard Cutting Tool Materials, China University of Mining and Technology (Beijing), Beijing 100083, China.

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Abstract: To solve the problem of uniform high-quality sintering of large-diameter polycrystalline diamond compact (PDC) cutting tool material on a cubic press, the design of a high-temperature, high-pressure (HTHP) sintering cavity assembly structure of a cubic press is optimised. PDC cutting tool materials with Φ62mm were successfully sintered at a pressure of 5.5–5.8 GPa and a temperature of 1550–1650 ℃. The microstructure and phase composition of PDC samples were

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detected by scanning electron microscopy, X-ray diffraction, and Raman spectroscopy. The microhardness, flexural strength, interfacial shear strength, wear resistance, and heat resistance of the samples were tested by a Vickers hardness tester, universal testing machine, and an abrasion ratio tester, and their uniformity was analysed. The test results show that the microhardness of Φ62 mm PDC is 86.25 GPa, which is 13.34% higher than that of the conventional PDC cutting tool material on the market; the bending strength is 1398.6 MPa; the interfacial shear strength is

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2690.4 MPa; and the wear ratio is 29.8  104 with only an 8.09% decrease from the peripheral point to the central point. The wear resistance is basically uniform in the radial direction, indicating that the HTHP sintering process and the structure of the sintering cell assembly are reasonable, and the temperature and pressure field distributions inside the high-pressure sintering cavity are uniform, thereby realising uniform, dense sintering of the Φ62 mm PDC. When the PDC sample was calcined at 750 ℃ for 2 min, the wear resistance was 29.8  104, which is 10.59% lower than the wear resistance at room temperature, and the sample had good heat resistance. Key words: Polycrystalline diamond compact; High pressure and high temperature; assembly; wear resistance; Heat resistance; strength

1 Introduction Polycrystalline diamond compact (PDC) is a composite super-hard material sintered by diamond powder and a WC/Co substrate at a pressure of 5–7 GPa and a temperature of 1500 –

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Corresponding authors: Fuming Deng，E-mail: [email protected]；

Xuefeng Yang，[email protected]

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1700 °C [1,2]. It not only has the high hardness, wear resistance, and thermal conductivity of diamond but also has the strength and impact toughness of its WC/Co substrate [3–5]. It is an ideal material for the manufacture of cutting tools, for the processing of difficult-to-machine materials such as nonferrous metals and hard and brittle nonmetallic materials [6–9], and for improving the cutting efficiency and cutting quality of the product to ensure a high-precision consistent product. Its implementation can significantly reduce the consumption of precious metals such as cobalt, tungsten, and niobium in high-speed steel and cemented carbide tools while reducing the energy consumption per unit of production. Especially, in the automotive and wood processing industries, PDC has become a high-performance alternative to traditional carbide tools [10–12], with a broad space for further development. With the advancement of cutting technology and the expansion of application fields, greater requirements for PDC size, quality, and performance uniformity and batch stability have been put forward. High-quality large-diameter PDC can not only improve processing quality and processing efficiency but can also meet manufacturing requirements of different cutting tool specifications, improve the utilisation rate and reduce the cost per unit area [13]. The manufacturing size and quality of PDC are closely related to the size of the high-temperature, high-pressure (HTHP) sintering cavity and the temperature field and pressure field distributions in the cavity [14], while the size of HTHP sintering cavity is affected by the tonnage of HTHP equipment and the quality of the tungsten carbide anvil. At present, PDC is sintered mainly by two ultra-high-pressure devices: a belt-type press and a cubic press [15]. The belt-type press is a single oil source press, and the oil cylinder is arranged in the lower part of the frame, which is convenient for using a large-diameter oil cylinder. The belt-type press enlarges the sintering cavity and provides a relatively uniform temperature field distribution, with a high-pressure utilisation rate, while producing a small deformation of the product. However, its annual ring mould system is complex, the consumption of tungsten carbide is high, and the production efficiency is low. Compared with the belt-type press, expanding the sintered cavity with the cubic press is difficult because of the tonnage restrictions of the equipment. It is not possible to produce oversized PDC tool materials like those of a belt-type press. Moreover, controlling the uniform distribution of the temperature field and pressure transmission in the cavity after expansion of the HTHP sintering cavity and achieving uniform and dense sintering of large-diameter PDC tool materials are urgent problems to be solved. However, the cubic press uses four nonheated tungsten carbide anvils and their support system to replace the annual ring mould system of the belt-type press, which offers low consumption of tungsten carbide, fast boosting and pressure relief, and high production efficiency. Therefore, studying the uniform and dense sintering of large-diameter PDC cutting tool materials on the cubic press is of great value. Based on the mature technology of the 60-MN cubic press, Φ62 mm PDC was successfully sintered by using the optimised design of the high-pressure synthesis cavity assembly structure, and its composition, structure, and properties were studied.

2 Experiment 2.1 Assembly structure design When sintering PDC, pressure-transmitting materials, heating materials, heat-insulating materials, insulating materials, and shielding materials will be used. The selection and assembly of these raw materials directly determines the quality of the sintered PDC composites. Especially, after the cavity is enlarged, the sintering time is prolonged, and the role of shielding materials in

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direct contact with the diamond powder is crucial [16] in not only preventing external impurities from entering the PDC during the sintering process but in playing an important role in the diffusion of cobalt in the PDC and the growth and bonding of the diamond particles. Therefore, the selection of an appropriate shielding material is crucial for HTHP sintering process stability and quality of the entire PDC. The working principle of the cubic press entails simultaneous pressure and pressure relief of six tungsten carbide anvils on a central cube assembly block [17]. A schematic of the cubic press assembly showing the six opposite anvils and the cube assembly in the middle is shown in Fig. 1. In this study, the assembly structure of the molybdenum (Mo) cup and zirconium (Zr) double-layer shielding cup is adopted, and the PDC cutting tool material is sintered at high temperature and high pressure by indirect heating. Making the temperature and pressure distribution of the synthesis cavity uniform and meeting the Φ62mm PDC sintering requirements requires an optimised design of the sintered cavity assembly structure, as shown in Fig. 2 [18,19]. The synthetic block utilizes pyrophyllite and a dolomite liner as the external pressure transmission and heat preservation medium. This takes advantage of the characteristics of dolomite, which does undergo phase transformation under high temperature and high pressure, and reduces the influence of the pyrophyllite phase transformation on pressure transmission and improves the pressure distribution in the sintering cavity. The salt tube serves as the internal pressure medium. The salt tube and the salt sheet are in a liquid phase at high temperature; they help provide uniform pressure and heat preservation, reducing the pressure gradient of the synthesis cavity and making the HTHP fields of the synthesised PDC material more uniform and stable. The conductive steel ring consists of a large-diameter thin-wall structure. The core is filled with dolomite and the pyrophyllite ring is placed on the periphery to achieve conductive insulation at both ends and to avoid burning the tungsten carbide anvil.

Fig. 1. Schematic of the cubic press assembly showing the six opposite anvils and the cube assembly in the middle.

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Fig. 2. Schematic of the cell assembly used in the HTHP experiments.

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1: pyrophyllite; 2: dolomite tube; 3: carbon disc; 4: salt tube; 5: molybdenum cup; 6: zirconium cup; 7: titanium sheet; 8: conductive steel ring; 9: dolomite core; 10: cemented carbide substrate; 11: diamond powder; 12:

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pyrophyllite ring.

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2.2 Experimental methods

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The starting materials utilised in this study were diamond powder (with a particle size of 5/10 μm; D50: 7.5 ± 0.75 μm), cobalt powder (with a particle size of 1–3 μm and a purity a 99.99%), and a WC/16%Co cemented carbide substrate [20]. The HPHT experiments were performed in a 60-MN large-volume cubic press. The cell assembly used in the HPHT experiments is shown in Fig. 2. During the HPHT synthesis experiments, the cell pressures ranged from 5.5 to 5.8 GPa and temperatures varied from 1550 ℃ to 1650 ℃ with a duration time of 20 min. During the experiment, the sintering pressure was calibrated using Bi (2.55 GPa, 7.7 GPa), Tl (3.7 Gpa), Ba (5.5 Gpa), and the temperature was measured using a platinum rhodium 30-platinum rhodium 6 (type B) thermocouple. The HPHT sintered structure of PDC is shown in Fig. 3, which shows the dynamic process of HPHT sintering for the Co, diamond, and WC/Co substrate. During the HTHP sintering process, the cobalt in the cemented carbide melts into a liquid phase and diffuses into the diamond powder layer and sweeps across the entire diamond layer. The diamonds grow together in the process of melting and recrystallisation. Through precise control of sintering conditions and processes during the experiment, effective control of the graphitisation of the diamond surface and uniform diffusion movement of the cobalt liquid were obtained, thereby achieving diamond– diamond bonding and uniform sintering. The sintered PDC sample was subjected to a grinding process and polished to make the surface of the sample mirror-like. The experimental sintered Φ62 mm PDC sample is shown in Fig. 4. The total thickness of the sample was 2.0 mm, and the thickness of the diamond layer was 0.5 mm. The phase and structure of the PDC samples were analysed by scanning electron microscopy (SEM), X-ray diffraction (XRD), and Raman spectroscopy. The hardness of the polished surface was tested using a Vickers hardness tester. The wear resistance of the PDC was measured by grinding the PCD layer with a standard silicon carbide grinding wheel according to the industry standard JB/T3235-2013 and using a JS71-A type wear ratio measuring instrument. Interface shear strength and flexural strength tests were performed on a CMT4305 electronic universal testing

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Fig. 3. Schematic of the structure for HPHT sintering of PDC, showing the dynamic process of HPHT sintering for

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Co, diamond, and WC/Co substrate.

3 Results and discussion

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3.1 SEM analysis

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Fig. 4. Φ62 mm PDC.

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Scanning electron micrographs of the starting diamond powder and PDC samples are shown in Figs. 5(a) and 5(b). The corresponding energy dispersive X-ray spectroscopy measurements on different regions shown in the SEM image of the PDC sample are shown in Figs. 5(c) and 5(d). According to the energy spectrum results, the white portion of the figure is a metal binder phase, and the black portion is diamond. It can be seen from the figure that the sample is dense and crack-free and that the diamond grains are closely arranged. Most of the diamond powder has been sintered and joined together. The direct bonds are diamond–diamond bonds, and the binder metal has been displaced with respect to the trigonal grain boundary of the diamond grain to form a mass distribution. The binder metal was displaced with respect to the trinary grain boundary of the diamond grain to form a mass distribution, and a small part remains in the diamond grain boundary and has a thin vein-like distribution.

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Fig. 5. Scanning electron micrographs of the starting diamond powders (a) and PDC sample (b). (c) and (d)

of the PDC sample.

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3.2 XRD analysis

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Corresponding energy dispersive X-ray spectroscopy measurements on different regions shown in the SEM image

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Fig. 6. shows the XRD pattern of the PDC sample. It can be seen from the figure that the sintered PDC sample contains the binder metal cobalt and the tungsten carbide phase in addition to diamond. This indicates that, during the PDC sintering process, the metal cobalt in the cemented carbide matrix melts into a liquid phase to diffuse and penetrate the diamond layer, while the tungsten carbide in the cemented carbide will also dissolve in the cobalt solution and infiltrate into the diamond layer. The binder metal phase is uniformly distributed around the diamond and at the grain boundary, which promotes diamond–diamond bonding, and it penetrates into the gap between diamond particles, making the PCD more dense and improving wear resistance and thermal stability. No graphite phase was found in the sample, indicating that it was sintered in the stable region of diamond. During the sintering process, graphitisation of the surface of the diamond powder completely converted the diamond under the catalytic action of the metal cobalt to form diamond–diamond bonds.

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Fig. 6. PDC XRD pattern.

3.3 Raman analysis

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To further verify the composition of the synthesised PDC samples, Raman spectroscopy was performed on the synthesised PDC samples because of the higher sensitivity of graphite to Raman spectroscopy. Fig. 7 shows a Raman spectrum of the PDC sample. It can be seen from the figure that there is only a 13327.66 cm-1 diamond characteristic peak in the sample, and there is no characteristic peak for graphite. In the HTHP sintering process, graphitised carbon on the diamond surface is all converted into diamond, forming diamond–diamond bonds.

Fig. 7. PDC Raman spectrum.

3.4 Mechanical properties

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With the expansion of the synthesis cavity, pressure gradients and temperature gradients along the inner edge and in the central region of the synthesis cavity inevitably arise. Ensure that all points inside the cavity are in the same sintering condition, so that the quality of the whole PDC is uniform, is key for sintering large-diameter PDC composites. Microhardness and wear resistance are important indicators used to measure the quality of PDC tools, directly affecting the processing effect and service life, and are also important indicators for evaluating the uniform sintering of PDC. It is therefore important to investigate the hardness and wear resistance of PDC materials and the uniform distribution from the centre to the edge. In this study, Vickers microhardness and wear resistance tests were performed on the sintered PDC samples in the radial direction. During the experiment, five different positions were selected from the centre of the circle, O, along the radius R direction to perform the hardness test, as shown in Fig. 8. The hardness tester used in the experiment was an FV-700 Vickers hardness tester. The loading pressure was 98 N, and the pressure holding time was 15 s after the pressure head was pressed into the sample. The values reported are the average values of three measurements for each test point. The hardness test results are shown in Fig. 9. It can be seen from the figure that the hardness of the edge point is up to 89.7 GPa, the hardness of the centre point is 81.26 GPa, and the average hardness is 86.25 GPa, which is 13.34% higher than the hardness of the conventional tool PDC composite on the market. It can also be seen from the figure that the hardness of the PDC sample gradually decreases from the edge to the centre, similar to the radial distribution of pressure in the sintered cavity. The hardness of the centre point relative to the edge point decreases by 9.4%, indicating that the pressure gradient in the high-pressure chamber is small and that the pressure is evenly distributed.

Fig. 8. Φ62mm PDC radial hardness test point.

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Fig. 9. Φ62mm PDC loading pressure (98 N) radial hardness test result. Inset: Optical micrograph of the Vickers

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3.4.2 Bending strength

The bending strength R of the PCD layer was tested on a CMT4305 electronic universal

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testing machine by using a three-point bending method. The sample size was 6  2  0.5 mm, and the loading speed was 0.5 mm/min. Table 1 lists the calculation results according to R = (3FL)/(2bh2),

(1)

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where F is the destructive load (in newtons), L is the span (in millimetres), b is the width (in

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millimetres), and h is the thickness (in millimetres).

It can be seen from Table 1 that the sample has a high flexural strength and that the average flexural strength reaches 1398.6 MPa.

Sample

1

2

3

4

5

1348

1389

1376 1398.6

1423

1457

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Bending strength (MPa) Average value (MPa)

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Table 1. Bending strength test results

3.4.3 Interfacial bonding strength

The PDC sample was laser-cut into the shape shown in Fig. 10, and an interface shear strength test was performed on it with a CMT4305 electronic universal testing machine. The interfacial shear strength τ is calculated by using τ = F/A,

（2）

where F is the destructive load (in newtons) and A is the area over which the force is applied (in square millimetres). The calculation results are listed in Table 2.

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Fig. 10. Schematic of the shearing experiment.

Sample Interface shear strength

(MPa)

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2

2613

2640

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Average value (MPa)

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Table 2 Interface shear strength test results

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4

5

2687

2743

2769

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5

14

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16

2690.4

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Heat resistance (times) Average (times)

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Sample（Quenching at 750 ° C）

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Table 3 PDC interface quenching and crushing experiment results

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2

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13.6

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During the shear strength test of the PDC interface, when a breaking load was applied, the PDC collapsed into a block form; the small pieces that collapsed did not all peel off along the interface joint, with most of them peeling off from the side of the cemented carbide, indicating interface bonding. The strength was found to be higher than the strength of the cemented carbide itself. It can be seen from Table 3 that the PDC is quenched at 750 ℃ for an average of 13.6 times, and the layer is cracked after the crush test, showing good interfacial bonding performance. 3.5 Wear resistance

According to the point-taking method of Fig. 8, a PDC wear resistance sampling test was performed in the radial direction. For the first position, the wear surface was over the centre of the circle; for the second position, the wear surface was over the centre [(1/4)R]; for the third position, the wear surface was at (1/2)R; for the fourth position, the wear surface was at (3/4)R; and for the fifth position, the wear surface was at the edge portion of the PDC disc. The wear ratio test results are given in Table 4. It can be seen from the table that the Φ62 mm PDC material exhibits excellent wear resistance and that the wear resistance from the edge to the centre gradually decreases in the radial direction. The wear resistance of the edge point is up to 30.9  104, and the wear resistance of the centre point is the lowest at 28.4  104, with the average being 29.8  104, so the wear resistance of the centre point relative to the edge point is only 8.09%. The radial wear resistance is basically uniform, indicating that the HTHP sintering process and the structure of the sintering cavity are reasonable. The pressure field of the internal temperature field

Journal Pre-proof of the cavity is evenly distributed, and uniform and dense sintering of the Φ62mm PDC material is realised. Table 4. PDC wear resistance test results

Sample

Wear resistance (104)

Wear resistance at 750 ℃ for 2 min (104)

28.4

25.2

2

29.2

26.1

3

30.1

26.8

4

30.6

5

30.9

Average

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27.4

To investigate the comprehensive heat resistance of the PDC material, the sample was placed

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in an electric resistance furnace and heated to 750 ℃ in an air atmosphere for 2 min. After

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cooling to room temperature, the wear resistance of PDC samples was tested after heat treatment. The test results are given in Table 3. The test results show that the edge point wear resistance is

4 Conclusion

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27.9  104, the centre point wear resistance is 25.2  104, and the average wear resistance is 26.7  104, which is 10.59% lower than the normal temperature wear resistance. Therefore, Φ62mm PDC sintered in the experiment exhibits excellent heat resistance.

1. Through the design of the assembly structure of the HTHP sintering cavity, Φ62 mm PDC material was successfully sintered by a 60-MN large-volume cubic press at a pressure of 5.5 to 5.8 GPa and a temperature of 1550 ℃ to 1650 ℃. The sample has no defects such as delamination, cracks, and uneven thickness of the diamond layer. The Vickers hardness reached 86.25 GPa, the flexural strength was 1398.6 MPa, the interfacial shear strength was 2690.4 MPa, and the wear resistance was 29.8  104. Superior mechanical properties and excellent wear resistance were obtained. 2. The sample is dense and crack-free, and the diamond grains are closely arranged. Most of the diamond powder has been sintered and joined together, forming direct bonds through diamond– diamond bonds. The binder metal is squeezed to the trigonal grain boundary of the diamond grain to form a mass distribution, and a small part remains in the diamond grain boundary and has a thin vein distribution. 3. Wear resistance of the Φ62mm PDC material is only 8.09% from the edge to the centre point, and the radial wear resistance is basically uniform. This indicates that the HTHP sintering process

Journal Pre-proof and the assembly structure of the sintering cavity are reasonable. The temperature field and pressure field distributions inside the sintering cavity are uniform, and uniform and dense sintering of Φ62 mm PDC material is realised. 4. The PDC sample was calcined at 750 ℃ for 2 min, and the wear resistance was 26.7  104, which was 10.59% lower than the normal temperature wear resistance. The Φ62 mm PDC sintered in the experiment has excellent heat resistance.

Acknowledgement: Colleges and Universities High-level Talent Cross Training Plan of Beijing - Practical Training Projects (No.2018110750311).

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References

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Journal Pre-proof Declaration of interests

☒ The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

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may be considered as potential competing interests:

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☐The authors declare the following financial interests/personal relationships which

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Graphical abstract

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Highlights

(1) The design of an HTHP sintering cavity assembly structure of a cubic press was optimised. (2) Φ62mm PDC cutting tool materials were successfully sintered on a cubic press.

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(3) Performance and uniformity of Φ62mm PDC tool materials were evaluated.