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Vol. 8. Issue 6.
Pages 5823-5832 (November - December 2019)
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Vol. 8. Issue 6.
Pages 5823-5832 (November - December 2019)
Original Article
DOI: 10.1016/j.jmrt.2019.09.052
Open Access
Microwave synthesis of B4C nanopowder for subsequent spark plasma sintering
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D. Davtyana, R. Mnatsakanyana, L. Liub, S. Aydinyana,b,
Corresponding author
sofiya.aydinyan@ttu.ee

Corresponding author at: Tallinn University of Technology, Ehitajate tee 5, 19086, Tallinn, Estonia.
, I. Hussainovab
a A.B. Nalbandyan Institute of Chemical Physics NAS RA, P. Sevak 5/2, Yerevan, 0014, Armenia
b Tallinn University of Technology, Ehitajate 5, Tallinn, 19086, Estonia
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Table 1. SPS parameters and mechanical properties of B4C specimens.
Table 2. Comparative overview of the spark plasma sintered B4C without additives.
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Abstract

Utilization of microwave-assisted (MW) synthesis and subsequent spark plasma sintering as an efficient and rapid synthetic route toward the preparation and consolidation of ultrahard B4C boron carbide without additives is reported. Magnesium dodecaboride (MgB12) and carbon were used as raw materials for stepwise MW synthesis of B4C at irradiation power of 900W. The comprehensive analytical studies showed that after few minutes of microwave irradiation of reactive mixture single phase nanoparticles of boron carbide (40–50nm) covered by carbon nanolayer are formed. Optimum sintering parameters for the powder compaction were revealed and dense specimens (>99%) with hardness of around 35GPa and substantially improved fracture toughness of 5.7MPam1/2 were produced from nanosized B4C powder without any additives. Erosive wear behaviour of B4C against silica particles impact studied at room temperature demonstrated a high erosion resistance for the fully dense compacts sintered at 1900°C.

Keywords:
Boron carbide
Nanopowder
Microwave assisted synthesis
Spark plasma sintering
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1Introduction

The spectrum of superior and unique properties of advanced and refractory boride and carbide ceramics generated the interest in the synthesis of high-quality powders, fibers, films, compacts for applications where excellent durability, improved performance, unique design capability and cost efficiency are explicitly utilized [1,2]. Boron carbide (B4C) is one of the hardest materials (HV 29.1GPa) [3] of a strategic importance due to combination of low density (2.52g·cm−3) [3], high Hugoniot elastic limit, good chemical resistance [4], high neutron absorption cross-section (600 barns) [5], and excellent thermoelastic and thermoelectric properties [6]. The main factor limiting its wide use is a low fracture toughness and a lack of plasticity. B4C is an essential material for cutting tools, ceramic bearings, grinding, lapping, polishing, hot pressing and sintering of hard and abrasion resistant parts with light weight, metallurgical refractories with high corrosion and oxygen resistance, moderators, blast nozzles, and nuclear technology reactor control rods, etc. The extreme hardness of boron carbide ensures its outstanding wear and abrasion resistance and, consequently, its application is expanded to nozzles for slurry pumping, grit blasting and water jet cutters [7]. Thin films of boron carbide are especially efficient as protective coatings in electronics [8].

Moreover, B4C serves as an important precursor component for the production of boron nitride and transition metal diborides [9,10]. As boron carbide is a p-type semiconductor, it considered as a potential candidate material for the electronic devices (thermocouple, diode and transistor devices) that can withstand the high service temperatures [11].

Commercially, boron carbide is produced by the reduction of boron anhydride (or acid) with carbon or magnesium in the presence of carbon black [12,13]. Other routes for preparation of boron carbide powder include reactive synthesis in gas phase [7], synthesis from polymer precursors [14,15], liquid and/or solid phase reactions [16], and microwave (MW) synthesis from boron acid [2]. The approach of MW synthesis has been extensively used for the preparation of various types of carbides, borides, nitrides, halides from elementary mixtures or corresponding oxides [17]. The method of MW heating as a rapidly developing process is essential energy-efficient routine for the synthesis of nanocrystalline powders [2]. Microwave ovens are used as a radiation source with a frequency of 2.45GHz at a maximum power range of 1–2.5kW.

However, in spite of its high temperature strength and well-elaborated methods of fabrication, the applications of B4C are limited due to difficulties in densification of the ceramic possessing high melting point, low self-diffusion coefficient and high vapor pressure. Usually, high sintering temperatures (>2000°C) or sintering aids (carbon, SiC, TiB2, Al2O3) are required for its densification affecting the mechanical properties of the sintered ceramic to a great extent. Recently, several attempts were made to apply spark plasma sintering (SPS) technique for the fabrication of high density B4C specimens [18–20]. It was supposed that microstructure characteristics and mechanical properties of boron carbide can be noticeably improved by selectively chosen synthesis and consolidation methods. The purpose of the present study is utilization of the microwave heating method to synthesize the nanocrystalline boron carbide using a stoichiometric mixture of magnesium polyboride and carbon in a quartz reactor placed in a microwave oven. In addition, the compaction conditions via spark plasma sintering (SPS) technique of the microwave synthesized boron carbide powder without additives are examined and the mechanical properties of dense bulks are analysed.

2Material and methods2.1Microwave synthesis

Amorphous MgB12 (99.0%, magnesium ∼15%) and carbon powder (Vulcan XC-72R, Cabot Co) were used as the precursors for the synthesis of B4C boron carbide. Magnesium dodecaboride (MgB12) served as both the source of boron and reducer; i.e. Mg purifies the carbon powder from the adsorbed oxygen(C(O)). A stoichiometric ratio of the elements in the initial mixture was calculated taking into account the MgB12+3C(O)=3B4C+Mg(O) equation.

The mixture of powders containing 2g of MgB12 and 0.47g of C (2.5wt.% higher than stoichiometric ratio) was weighed and carefully mixed in a quartz cup for two hours using a magnetic stirrer. Afterwards, the mixture for better degasifying was placed in a quartz flow reactor. A quartz lid containing tubes for gas inlet and outlet was mounted at the top of the reactor, which was purged with 25ml min-1 flow of high purity (99.999%) helium at a room temperature for 2h. Then the reaction mixture has been collected in the bottom of quartz reactor and tube was vertically inserted into the oven through an opening. To avoid rapid reaction and strong gas release, the reactor with the mixture was irradiated in five successive steps at 5, 10, 20, 30s for 900W at each step. Subsequently, the mixture was subjected to microwave heating at 900W to white-hot glowing for 600s. Average temperature of microwave heating was measured to be 1150°C by infrared thermometer (Dostman HT 1800). Continuously flowing helium was used to protect materials from oxidation during the synthesis. During cooling, the gas flow was kept for 2h. Then the product was maintained inside the reactor at room temperature for 24h for the deactivation of surface. To ensure the complete removal of byproducts (Mg(O), B2O3 and other impurities), the final product was leached with 5% NaOH and 5% hydrochloric acid solutions and washed with deionized water for several times.The residue was filtered and dried in an oven at 105±0.5°C for 12h.

2.2Characterization

The phase composition of the synthesized powder was examined by X-ray diffraction (XRD; D5005, Bruker, USA). Step-scan data were collected with CuKα radiation (λ=1.5406Å) at a step size of 0.02◦(2θ) and a scanning rate of 4°min−1. Morphologies and microstructures of the samples were analysed with the help of field-emission scanning electronic microscope (FE-SEM, Zeiss Evo MA15, Germany) equipped with energy dispersive spectroscopy (EDS).

The densities of the as-sintered samples were measured by Archimedes' technique using distilled water medium (Mettler Toledo ME204, Switzerland).The theoretical density was calculated applying the rule of mixtures. The Vickers microhardness and indentation fracture toughness were measured using hardness tester Indentec 5030SKV applying 5kgf force for dwell time 10s. At least 20 indentations were performed to obtain the average hardness value and the standard deviation.

2.3Spark plasma sintering

The B4C powder was compacted in a graphite die of 20mm in diameter lined with graphite foil and consolidated by spark plasma sintering technique (KCE®-FCT HP D 10-GB, FCT Systeme GmbH, Germany) in vacuum at temperature of 1750–1900°C with simultaneous application of 50MPa pressure for a dwell time of 5–10min. The heating rate was set to 100°C/min (Table 1).

Table 1.

SPS parameters and mechanical properties of B4C specimens.

No  Temperature, °C  Dwell time, min  Archimedes density, g/cm3  Relative density, %  Vickers microhardness, HV5, GPa 
1750  2.251  89  – 
1800  2.321  92  22.5±4.1 
1900  10  2.499  >99  34.5±2.3 
2.4Erosive wear test

Erosion testing was conducted with the help of a centrifugal four-channel accelerator described in details elsewhere [21,22]. The mass of erodent SiO2 particles charged into a hopper was 6kg for running-in period and 6, 10 and 15kg afterwards. Silica sand with particle size of 0.1–0.6mm was used as the erodent travelling at velocities of 30, 50 and 80 m⋅s−1 under an angle of impingement of 30° at a room temperature. The erosion rate was determined as the volume loss of the target sample per mass of erodent particles (mm3kg−1). The spark plasma sintered specimens were polished with an abrasive paper to a surface roughness (Ra) of about 0.1μm. To quantify the weight loss, the specimens were ultrasonically cleaned in ethanol and weighed before and after the test to the nearest 0.1mg using GR-202 A&D Instruments balance.

3Results and discussion

The XRD pattern of the dried samples identified the peaks representing the data lines of boron carbide (B4C, PDF #35-0798) from JCPDS database and a broad and low-intensity line for the graphitic carbon (PDF #41-1487) at ∼26° (Fig. 1a). The SEM image of MW synthesized powder demonstrates the presence of particles of well-defined grain boundaries with average particle size of 300nm (Fig. 2, area A) and agglomerated particles with an average diameter of a single particle of ∼40–50nm (Fig. 2, area B).

Fig. 1.

XRD patterns of MW synthesized B4C boron carbide: (a) before sintering, (b) after sintering.

(0.1MB).
Fig. 2.

SEM images of B4C powder after MW synthesis (a, b, c, d-different magnifications).

(1.14MB).

X-ray diffraction analysis of the SPSed materials regardless of sintering temperature revealed the same data lines of boron carbide (B4C, PDF#35-0798) (Fig. 1b). After the SPS process, the intensity of boron carbide diffraction peaks is increased and the width at a half-maximum of boron carbide peaks is substantially narrowed.

The broadening of diffraction peaks within the 30–80° angular range allows using the Scherer equation for the estimation of the average crystallite size of the B4C phase, which makes ∼18nm. This discrepancy of average crystallite size and particle diameter evaluated by SEM can be related not only to the nano-sized particles, but also to the presence of increased amounts of defects in the nanoscale particles, which contributes to the additional broadening of XRD lines [23].

The EDS analysis (Fig. 3) testifies presence of two slightly different compositions of the MW produced particles, both of which correspond to B4C of different ratios between boron and carbon. In the object “1214”, which corresponds to nanocrystals of 300nm average size (Figs. 2 and 3, area A), carbon/boron ratio is higher than one, in contrast to the object “1213” (40–50nm, Figs. 2 and 3, area B), where carbon/boron ratio is lower than one. It is reasonable to assume that 40–50nm nanoparticles match to B4C, and nanograins/nanocrystals with average size of 300nm are agglomerated boron carbide covered with free carbon.

Fig. 3.

EDS analysis of B4C powder after MW synthesis (Green-1213, Blue-1214) (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article).

(0.23MB).

It is known that efficiency of sintering depends, among other factors, on particle size [24], herewith fine particles provide a higher efficiency of sintering. From this point of view, the MW assisted method allows to synthesize nanoparticles with a narrow size distribution, which may ensure high density of the produced materials. The second strongly influencing factor is the presence of a binder phase; in this case, a thin layer of carbon may play an important role [25]. In addition, carbon decreases the melting point on the B4C–C interface to the eutectic point intensifying material transport. Free carbon in the boron carbide powder migrates within the grain boundaries during sintering and agglomerates as graphite inclusions at the grain triple points.

According to the available literature data presented in Table 2, the sintering process of B4C powder is mainly affected by the temperature of sintering. Depending on the preparation method, particle size and purity of the B4C powder, the densification is recommended to be performed in a temperature range of 1600–2100°C. Materials produced at lower temperatures (1600–1800°C) were of a high porosity (up to 10%) and, therefore, were considered as irrelevant for testing of mechanical properties. In the current study, the moderate temperature range was selected (1750–1900°C). While compaction pressure is kept at 50MPa for all experiments, the differences in relative density and mechanical properties can be attributed to the sintering temperature and the dwell time. Particularly, an increase in temperature from 1750 to 1900°C resulted in 10% increase in density as demonstrated in Table 1.

Table 2.

Comparative overview of the spark plasma sintered B4C without additives.

Reactants  Process parameters  Average grain size  Relative density, %  Hardness, GPa  Fracture toughness, MPam1/2  Reference (year) 
Synthesis of B4C from elemental powders by field activation using (SPS)  1800°C, 70MPa, 10min, 200°C/min  From 100nm to several micrometers  90  –  –  28 (2005) 
Sub-micrometrer sized commercial boron carbide  1750°C, 88MPa, 5min  2μm  99.2  27.45  3.61  29 (2007) 
Mixed B3.5C, B4.0C and B4.5C synthesized from carbon and boron  1900°C  –  95  –  –  30 (2007) 
Ball milling of boron (0.5ìm) and carbon  1900°C, 20MPa, 26min  –  95  –  –  31 (2009) 
B4C powder HS grade supplied by H.C. Stack  2050, 6min/10min, 32MPa, 50°C/min  4.05±1.62μm  98/100  –  –  32 (2010) 
B4C HP grade  1800°C, 50MPa, 5min  2.95μm  97.90  32  4.3  33 (2010) 
B4C HS grade  1770°C, 50MPa, 5min  1.77μm  99.86  32.5  4.5  33 (2010) 
B41800°C, 50MPa, 10/15min  2.4μm  96/100  33.3/37.2  3.1/2.8  18 (2014) 
Commercial B4C powder (Mudanjiang Diamond Boron Carbide Co., Ltd., China)  1931°C, 35.3MPa, 1–2min  2.36μm  99.2  –  –  34 (2016) 
15min HEBM of B+C mixture  1950°C, 60min, 50MPa  ∼3μm  98.1±0.4  36.34±0.32  4.34±0.26  35 (2017) 
B4C from amorphous boron (74μm) and GNP (5μmx5nm)  1600°C, 50MPa, 50°C/min, 10min  sub-micron grains  96  21.1  Impossible to measure because of brittleness  36 (2018) 
B4C obtained by carbothermic reduction of boron oxide/boric acid  2100°C, 40MPa, 20min, 100°C/min  3.33μm  99.66  –  –  19 (2018) 
Commercially available B4C powders (97.1% purity, Shanghai ChaoWei Nanotechnology Co., Ltd., China)  40MPa, 1900°C, 100°C/min, 20min  <3.13μm  93.87±0.53  26.4±4.3  3.15±0.23  24 (2018) 
B4C powder H.C. Starck (grade HD20, Germany)  1650°C, 100MPa, 5min, 200°C/min  591±26nm  98±30±–  37 (2018) 
B4C (99.9%, 1ìm, Shanghai Xianxin New Material Technology Co., Ltd)  1850°C, 80MPa and 5min  3.65±0.14μm  98.5  33.5  5.0  38 (2018) 
B4C by microwave synthesis  1900°C, 50MPa, 10min, 100°C/min  50–300nm  >99  34.8±2.3  5.7±0.6  Present work 

An increase in density (or decrease in porosity level) with an increase in sintering temperature is clearly evident from the SEM micrographs (Suppl. Fig. 1). Micrograph of B4C processed at 1800°C indicates the initial stage of sintering, discretely densified regions with interconnected pores and formation of interparticle bonds (Suppl. Fig. 1a). Contacts between the powder particles are imperfect in nature, the cleavage passes along the intergrain boundaries, which indicates their weak connection. Suppl. Fig. 1b describes a structure formed under more intense sintering conditions (1900°C, 10min) and confirms the presence of deformation twins. The grain interparticle contact has a larger area and the content of consolidated grains is incomparably higher as compared with structure obtained at 1800°C.

Based on the microstructural and parametric studies, the optimum temperature for compaction was settled to 1900°C applied during 10min at a pressure P=50MPa (specimen 3). Geometrical and Archimedes densities of B4C compacts consolidated at optimum conditions were measured as 2.510 and 2.499g·cm−3, respectively. Accordingly, the relative density makes >99%.

Microhardness measured by Vickers indentation method showed that HV5 of B4C makes 34.5±2.3GPa. The hardness values for the nanostructured B4C are somewhat higher as compared to the hardness of the material prepared by conventional methods [23]; however, it is close to the value of 36.4GPa reported in Ref. [26] for spark plasma sintered B4C, which is apparently attributed to the maintained nanostructure at the fast SPS processing. Indentation fracture toughness (IFT) was determined on the base of radial cracks arising from the corners of the indents. IFT of the sample 3 calculated by Median, Evans and Palmqvist methods gave values of 3.7MPam1/2, 5.1MPam1/2 and 5.7MPam1/2, respectively. These values outperform to the values reported in the literature [18]. The IFT of the fully dense B4C sample was measured as 2.8MPam1/2 and increases up to 4.3MPam1/2 corresponding to 94% density [18]. IFT values of the full dense samples produced in the current study are close to the values reported for B4C sintered with SiC additives [27].

Micrographs of fracture surfaces of boron carbide (sample 3) are shown in Fig. 4. The fracture surface of the completely dense sample shows predominantly mixed brittle fracture modes: transcrystalline and intercrystalline mechanisms (Fig. 4c); however, the transgranular fracture mode is predominant, which is confirmed by the presence of deformation twins (Fig. 4c,d).Twinning in B4C is reported to occur along rhombohedral planes of the types {1011} and {1015} [24,26]. SPSed samples are found to exhibit increased density of twin structures with an increase in duration of sintering. Acceleration of densification process by electric field and simultaneous application of load during 10min of holding period assists promotion of diffusion and causes particle rearrangement and deformation contributing towards the evolution of twin structures (Fig. 4e,f). Fracture toughness infers that the twin boundaries act as an effective barrier to the crack displacement/development and contribute to material strengthening due to a lower energy interfaces as compared to the grain boundaries.

Fig. 4.

SEM images of fractured surface of B4C compacts (sample 3, Tsintering=1900°C).

(1.3MB).

The results of EDS analysis demonstrated the presence of B4C after SPS process, which certified that the main product is boron carbide, although trace amounts of oxygen also existed on the surface.

Combination of XRD, SEM, EDS analyses and evaluation of Vickers microhardness and indentation fracture toughness allowed to conclude that SPS sintering of MW synthesized boron carbide nanopowder ensures improved mechanical properties of the high density compacts produced at temperatures below 2000°C and with no any additives due to reduced defectiveness in the nanostructure of MW synthesized boron carbide.

Table 2 summarizes properties of the boron carbides densified by SPS technique [18,19,24,28–38].

Solid particle erosion of composite materials depends on many factors including mechanical properties of the target and erodent as well as the impact parameters. Erosion tests performed for boron carbide in Ref. [39] demonstrated outperformance of B4C over many existing hard materials used for abrasive waterjet nozzles. The erosion tests carried out for the sintered B4C impacted by silica erodents showed the effect of erodent velocity on the erosive wear rate and the mode of damage. Fig. 5 displays the volumetric erosive wear rate of the spark plasma sintered B4C specimens recorded during the centrifugal solid particle erosion test at a room temperature. Comparative analysis of erosive wear showed that the material sintered at a temperature of 1900°C (sample 3, Suppl. Fig. 2) exhibits the highest erosion resistance (exhibiting 6 times lower erosive wear rate at 80m/s erodent travelling velocity), while the sample 2 sintered at 1800°C is very sensitive to the change in erodent particles velocity and drastically increases with an increase in the velocity. In addition, sample 3 exhibited a low wear rate, which is comparable with the wear rate values of similar materials reported in literature [40]. Regardless the sintering temperature, the main erosive wear mechanisms operating at given conditions are similar, i.e., fracturing and/or fragmentation of carbide and removal of the whole ceramic grains due to intergranular cracking combined with some plastic deformation as indicated in Fig. 6 and Suppl. Fig. 2. From the micrographs, it can be seen that the appearance of the eroded bore surface shows obviously smaller pits and scratches on the sample 3 sintered at higher temperature.

Fig. 5.

Erosive wear rate of B4C sintered at different temperatures: sample 2 (Tsintering=1800°C), and sample 3 (Tsintering=1900°C).

(0.06MB).
Fig. 6.

SEM micrographs of B4C (sample 2) after the erosion test at 80m∙s−1 particles velocity.

(0.38MB).

In the light of aforementioned, MW assisted method allowed to synthesize nanoparticles with a narrow size distribution, which ensured high density of the produced materials in a moderate temperature regime. SPS process contributed to increase of the intensity and contraction of the width at a half-maximum of diffraction lines of boron carbide due to decreased amount of defects in the nanoscale particles. Free carbon in the boron carbide powder migrates within the grain boundaries during sintering intensifying densification process. Based on the microstructural and parametric studies, sample compacted at 1900°C during 10min at a pressure P=50MPa possess >99% relative density and higher Vicker’s microhardness as compared to the hardness of the B4C prepared by conventional methods attributed to the maintained nanostructure during SPS processing. IFT values of the fully dense samples produced from MW synthesized B4C in the current study were close to the values reported for B4C sintered with SiC additives facilitated by increased amount of twin structures.

4Conclusions

Microwave assisted synthesis allows preparation of B4C boron carbide nanopowder with an average diameter of the particles of ∼40–50nm directly from the stoichiometric mixtures of MgB12 and carbon. Subsequent spark plasma sintering guarantees the fabrication of the fully dense compacts (>99%) with an improved micro-hardness and an indentation fracture toughness of ∼35GPa and ∼5.7MPam1/2, respectively. The B4C bulk sintered at 1900°C under an applied pressure of 50MPa shows the least wear rate after erosion by silica sand at a room temperature. It was manifested that in addition to sintering temperature and duration, the method of nanopowder’ synthesis has a crucial influence on the structure-property characteristics of the compacted samples.

Conflicts of interest

The authors declare no conflicts of interest.

Acknowledgements

This work was supported by the State Committee of Science of Republic of Armenia18RF-114 (Raman Mnatsakanyan), Estonian Research Council under PUT1063 (I. Hussainova) and PSG220 (S. Aydinyan), MobilitasPluss postdoctoral researcher grant MOBJD166 (S. Aydinyan) and the Estonian Ministry of Education and Research (project IUT 19-29). Authors are greatly acknowledge Dr. Mart Viljus and Mr. Rainer Traksmaa for providing SEM and XRD analyses.

Appendix A
Supplementary data

The following is Supplementary data to this article:

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