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Original Article
DOI: 10.1016/j.jmrt.2019.09.042
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Available online 22 October 2019
Influence of TiC and Cr3C2 additions on the mechanical properties of a (W-Ti-Cr)C-Co sintered hardmetal
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Julian David Rubiano Buitragoa,
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judrubianobu@unal.edu.co

Corresponding author.
, Andres Fernando Gil Plazasb, Liz Karen Herrera Quinteroa
a Universidad Nacional de Colombia – Sede Bogotá – Facultad de Ingeniería – Departamento de Ingeniería Mecánica y Mecatrónica– Grupo de Investigación AFIS, Laboratorio de Fundición y Pulvimetalurgia – Cr 30 # 45-03. 111321 – Colombia.
b SENA, Centro de Materiales y Ensayos, Bogotá, 111511- Colombia
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Received 25 June 2019. Accepted 17 September 2019
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Tables (6)
Table 1. Sintered alloys.
Table 2. Semiquantitative elemental composition obtained by EDS.
Table 3. Analysis of variance (ANOVA) of the alloy composition on the hardness.
Table 4. ANOVA of the alloy composition on the fracture toughness.
Table 5. Analysis of variance (ANOVA) of the alloy composition on the volumetric loss.
Table 6. LSD test results of the hardness and volumetric loss.
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Abstract

TiWCrC-Co alloys were manufactured by conventional powder metallurgy processes in a vacuum alumina furnace. The alloys were sintered at 1550 °C, and the chemical composition was changed in order to evaluate its influence on the mechanical properties of the composite. The aim of this article is to explore the partial WC to TiC substitution effect and the microstructural changes of the alloys as a function of a Co and Cr3C2 grain growth inhibitor. Eight different alloys were sintered by changing the TiC [6–8 wt%], Cr3C2 [0.5–2 wt%] and Co [6–9 wt%] contents. The hardness was measured by the Vickers (HV30) method, and the fracture toughness was calculated by the Palmqvist method. High-Stress Abrasion Resistance tests (ASTM B611) were performed for all alloys. The Co and Cr3C2 contents influenced the mean grain size of the WC phase and thus the hardness of the alloys. The wear resistance showed a high dependence on the hardness and was not notably affected by the fracture toughness. The microstructure and phases were identified by scanning electron microscopy (SEM), Energy-dispersive X-ray spectroscopy (EDS) and X-ray diffraction (XRD). The Cr content did not exceed the solubility limit in the different alloys, and all TiC formed the TiWC2 phase and was homogeneously distributed, which hindered the Ostwald ripening process of the WC grains. Alloys with lower TiC and Cr3C2 contents developed the η phase that dispersed throughout the microstructure. TiC addition improved the wear resistance of the different alloys and is a good choice for manufacturing anti-wear components.

Keywords:
Hardmetal
Powder metallurgy
Cermets
TiWCrC-Co alloys
Anti-wear.
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1Introduction

Cemented carbides are a composite material known as hardmetal or CerMet, (Ceramic Metal). They are a group of sintered materials, made with hard and brittle refractory carbides from transition metals (like WC, TiC, TaC, Cr3C2 or Mo2C) in a ductile metal matrix that is commonly Co, Ni or Fe [1]. Powder metallurgy is the most common CerMet manufacturing process that can achieve high densities through liquid phase sintering [2,3].

Liquid phase sintering is understood to occur in three different steps. It starts with an initial particle rearrangement where a grain shape accommodation occurs, followed by a solution–reprecipitation process. Here the smaller grains dissolve in the liquid phase and reprecipitate in large grains; this mechanism is also called the Ostwald ripening process. Final microstructural coarsening involves the grain growth of the grain interfaces in contact with the liquid by diffusion. The reduction of grain interfacial energy is involved in all steps [4]. For that, a high solubility of the solid phase in the liquid and a very low wetting angle of the liquid in the solid are needed. The Co wetting angle in WC is 0° (this means that Co wets the WC grains thoroughly), and it is 25° in TiC which can promote the appearance of porosity in the final microstructure [5].

The solubility of WC in liquid Co is approximately 40% by weight, so high sintering times make the WC phase grow at a rate proportional to d3∼t[4,6]. Small TiC and Cr3C2 additions (near 2 wt%) to WC-Co hardmetals act as grain growth inhibitors [7–9], limiting the liquid phase solubility of the WC and mainly reducing the interfacial reactions in the Ostwald ripening process. This is due to the nanoscaled segregation layers of the inhibitors in the WC-Co interfaces [10]. Contents of grain growth inhibitors above the solubility limit within the Co phase tend to precipitate new phases. Additions of TiC near 18 wt% to a WC-Co cermet forms the fcc TiWC2 phase, which is harder than WC [11]. Increased TiC contents can form the rim-core microstructure based on grains with a core of TiC that is surrounded by TiWC2 coexisting with WC in the metal matrix [6]. All of those configurations are of great interest due to favorable enhancements in hardness and wear resistance of the alloy. If the Cr3C2 content is above its solubility within the alloy components, a Cr rich M7C3 brittle phase forms which is an undesirable situation [7,8,12,13]. The grain growth inhibitors have temperature ranges where the inhibition effect increases [14].

Although TiWC-Co and WCrC-Co carbides have been extensively investigated, a great deal of information related to the mechanical properties of TiWCrC-Co hardmetals has not been reported. The aim of this article is to study eight different TiWCrC-Co alloys by changing the TiC, Cr3C2, and Co wt% to evaluate the microstructural changes, in terms of grain size, phases and mechanical properties of the sintered samples. This information would provide several possible applications with improved cost effectiveness due to the lower volumetric cost of TiC and Cr3C2 with respect to that of pure WC-Co alloys.

2Experimental methods

Two 10 g samples were obtained for each alloy. The starting powders were milled for 5 h using a Fritsch planetary ball mill with a powder-to-ball ratio of 5:1, and 1 wt% of paraffin in hexane solution was added during the milling process. The milled powders were dried using a thermostatic bath at 80 °C for 2 h and then deagglomerated using a vibratory sieve with an 80 μm grid. The compacts were obtained at 200 MPa using a floating matrix and then sintered in a vacuum furnace with an Ar atmosphere added at 1350 °C. To avoid decarburization of the samples, graphite recipes were used for each one. The samples were sintered at 1550 °C for 90 min. During the heating step, the temperature was maintained at 400 °C for 20 min to ensure organic phase evaporation. The heating and cooling rates were 10 °C/min. During the cooling step at 900 °C, the samples were left inside the furnace without controlling the cooling rate and were cooled to room temperature.

The samples were polished using a 1 μm diamond suspension. The theoretical density was calculated through the rule of mixtures from the densities of WC, TiC, Cr3C2, and Co of the starting compositions (see Table 1). These values were then compared with the experimental density, which was measured by the Archimedes method using distilled water as liquid medium, to obtain the relative density. The porosity was estimated per the ASTM B276 standard using images obtained at 100× by optical microscopy. The hardness was measured by the Vickers method with 30 kgf, where 6 measurements were obtained for each sample. The fracture toughness (KIc) was calculated with Palmqvist method [15,16] using Eq. (1):

where  KIc is in MPam, HV30 represents the hardness measured at 30 kgf and ∑l represents the sum of the crack lengths generated at the corners of the Vickers indentation. The microstructure was studied with scanning electron microscopy (SEM), Energy-Dispersive X-ray spectroscopy (EDS), and X-ray diffraction (XRD). The samples were subjected to a wear test per the ASTM B611 standard. The grain size measurement was performed with digital analysis software using SEM-BSE images at 5000X from three different areas to obtain homogenous data set.

Table 1.

Sintered alloys.

Alloy  WC [wt%]  TiC [wt%]  Cr3C2 [wt%]  Co [ wt%]  R (% Co/% Cr3C2Porosity [ASTM B276] 
JR1  86  A04-B00-C00 
JR2  83  4.5  A04-B00-C00 
JR3  84  A06-B00-C00 
JR4  81  4.5  A04-B00-C00 
JR5  87.5  0.5  12  A06-B00-C00 
JR6  84.5  0.5  18  A04-B00-C00 
JR7  85.5  0.5  12  A06-B00-C00 
JR8  82.5  0.5  18  A06-B00-C00 
3Results and discussion

Table 1 shows the compositions of the alloys. A parameter referred to as “R” was calculated to quickly determined if the proportion of Co wt% of Cr3C2 wt% affects the response variables.

The porosity per ASTM B276 for the sintered alloys is reported in Table 1, where “A” represents the pores with a size <10 µm, “B” represents the pores with a size ranging from 10 µm to 25 µm and “C” represents the uncombined carbon (when free carbon is added); each category has five severity levels represented by number (starting with 00 which means no porosity). Samples with high R values and high TiC content tend to possess an increased porosity, which could be due to the Cr in the WC-Co alloy causing a reduction of approximately 107 °C, concerning to W-C-Co system, in the invariant reaction responsible for liquid formation [9]. This means that alloys with an increased amount of Cr form increased amount of liquid near to 1191 °C. Thus, the particle rearrangement is drastic for alloys with a high Cr presence. Finally increased amount of TiC make it difficult to reduce the porosity due to the reduced TiC wetting angle from the Co.

Fig. 1 shows that the mean relative density for the eight sintered alloys varied in a range of 0.4%. A 3D linear regression plane was added to the graph to show the behavior of the densification as the chemical composition varied, and make it easier to see that increased R values tend to improve densification. The higher densification values (red points) correspond to the JR4 alloy (left) and JR6 alloy (right). The JR4 alloy densification behavior can be explained by the higher content of Co, TiC and Cr3C2 than that of all other alloys, which implies that there was an increased amount of liquid Co present at the low temperatures as explained previously. On the other hand, the high densification of the JR6 alloy (which has low TiC and low CrC) can be explained by the formation of the eta phase (Co4W2C) as shown Fig. 2f. This result implies that this undesired phase improves densification during the initial steps because the eta phase amount is small and distributed throughout the microstructure. The decreased JR1 and JR2 alloy densification means that these alloys have an increased closed porosity.

Fig. 1.

Mean relative density for the sintered alloys.

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Fig. 2.

SEM-BSE microstructures of the sintered alloys, (a) JR1, (b) JR2, (c) JR3, (d) JR4, (e) JR5, (f) JR6, (g) JR7, and (h) JR8.

(0.99MB).

The microstructures of the sintered alloys are shown in Fig. 2, where WC faceted grains (white), TiWC2 grains (dark gray) and Co (black) can be seen, and the phases were confirmed by XRD patterns shown in Fig. 4. Samples JR5 and JR6 have the presence of η (eta) phase in the form of Co4W2C, as can be readily observed in Fig. 2e. Fig. 2f shows an increased amount of eta phase formation. The phase percentages of each sample were determined by digital image analysis of three SEM-BSE images, and the results are shown in Fig. 3. It is evident that the TiWC2 phase was proportional to the starting TiC content, and the alloys with eta phase had a dramatic reduction in free Co.

Fig. 3.

Mean phase percentage content of the sintered alloys calculated by digital image analysis.

(0.19MB).

Because all samples were sintered under the same conditions the presence of the η phase in the two alloys mentioned above could be explained by a carbon deficiency [17] that was influenced by the starting chemical composition. Alloys JR5 and JR6 had the lowest TiC and Cr3C2 additions (Table 1) among the alloys studied herein, meaning that the carbon in those compounds in solution within the alloy hindered decarburization of the samples that did not contain η phase. A remaining porosity is observed in all the alloys which is in contrast with the complete densification reported in [18] for a TiWCrC-Co alloy. Nevertheless, those results were obtained starting with pre-alloyed TiWC2 powders that had a 0° wetting angle with liquid Co. This could be due to the TiC + WC→ TiWC2 reaction in the sintered alloys occurring after particle rearrangement, which would lock gas in the pores due to low Ar solubility in Co after sintering.

Table 2 shows the semiquantitative elemental composition measured through EDS, reported as a function of the different phases identified by XRD (Fig. 4) and shown by arrows in Fig. 2. It was confirmed that most of the Cr was in solid solution in the Co phase, thus reducing the Co capacity to dissolve W. The ceramic phases also had small amounts of Cr in solid solution, which also varied considerably as a function of the starting Cr3C2 content.

Table 2.

Semiquantitative elemental composition obtained by EDS.

Phase [Alloy]  W (wt%)  Co (wt%)  Ti (wt%)  Cr (wt%) 
WC [JR1]  97.2  1.51  0.76  0.53 
Metallic [JR1]  36.23  57.12  0.78  5.87 
TiWC2 [JR1]  73.76  1.89  22.43  1.92 
WC [JR2]  96.2  2.41  0.99  0.4 
Metallic [JR2]  28.29  64.69  0.73  6.29 
TiWC2 [JR2]  71.45  2.16  24.81  1.58 
WC [JR3]  96.75  1.67  1.16  0.42 
Metallic [JR3]  45.73  47.83  1.98  4.46 
TiWC2 [JR3]  73.6  1.01  23.49  1.9 
WC [JR4]  93.65  4.03  1.78  0.54 
Metallic [JR4]  33.79  58.39  1.99  5.83 
TiWC2 [JR4]  67.21  2.03  29.2  1.56 
WC [JR5]  97.57  1.13  1.12  0.18 
Metallic [JR5]  43.28  51.96  2.55  2.21 
TiWC2 [JR5]  73.48  1.6  24.39  0.53 
Eta (η) [JR5]  74.74  22.06  1.1  2.1 
WC [JR6]  96.36  2.36  1.06  0.22 
Metallic [JR6]  35.57  61.46  1.2  1.77 
TiWC2 [JR6]  70.34  2.77  26.5  0.39 
Eta (η) [JR6]  73.31  23.52  1.32  1.85 
WC [JR7]  97.48  1.25  1.02  0.25 
Metallic [JR7]  50.69  46.15  1.22  1.94 
TiWC2 [JR7]  71.57  1.73  26.11  0.59 
WC [JR8]  97.17  1.54  1.11  0.18 
Metallic [JR8]  35.9  60.78  1.13  2.19 
TiWC2 [JR8]  69.95  2.91  26.69  0.45 
Fig. 4.

XRD patterns of the sintered alloys (a) Over large range (b) in a specific zone of the Co fcc phase.

(0.25MB).

The presence of Cr3C2 or any other carbide related to it was not identified in the XRD patterns, which confirms that the solubility limit was not exceeded. Samples with lower Cr3C2 starting content showed Co-fcc diffraction peaks that shifted to the left, as shown in Fig. 4b, where the red line represents the standard Bragg angle for Co-fcc and the black line represents the mean Bragg angle of the alloys with 2 wt% of Cr3C2. Thus the lattice parameter changed in the alloys due to an increased amount of W in solid solution, as confirmed in Fig. 5, where the large spheres (2 wt%Cr3C2) and the small spheres (0.5 wt%) showed the small and large lattice parameters respectively. This trend occurred because Co had an increased Cr content in solid solution, which decreased its capacity to dissolve W and vice versa.

Fig. 5.

Change in lattice parameter of Co fcc as function of Co and Cr Content (large spheres represent 2 wt% and small spheres represent 0.5 wt% starting Cr3C2).

(0.1MB).

The alloy chemical composition did not seem to have an apparent effect on the TiWC2 phase shape or size, while the WC phase had a high dependence on the mean grain size (Fig. 6a). The grain growth behavior differed for those two phases due to the low and high solubility of Ti and W in the liquid Co, respectively [19,20]; thus, Co saturation or low “R” values, tended to more efficiently inhibit the grain growth of the WC phase. Consequently, the reported nanoscale segregation layers in the WC grains due to the presence of grain growth inhibitors [10] must be influenced by the Co saturation.

Fig. 6.

Measured WC mean grain sizes (a) with respect to different sintered alloys, and (b) its influence on the hardness.

(0.25MB).

In addition to the “R” ratio, Fig. 6a shows that the TiC content also influenced the WC grain size. As shown in Fig. 3, the TiWC2 phase amount was dependent on the starting TiC content, which means that the TiWC2 presence hindered the Ostwald ripening process of the WC grains increasing the hardness of the alloy. Even if the standard deviation of the WC grain sizes is very similar, the high quantity of grains analyzed per sample (nearly 10,000) indicates that the hardness was very sensitive to the mean grain size. The mean hardness measured for the sintered alloys is shown in Fig. 6b, where it can be seen that the hardness obeys the Hall-Petch relation in terms of the WC grain size; as the amount of TiWC2 increased, the hardness of the alloy increased since TiWC2 is approximately 400 HV harder than the WC [1]. However, the alloys with η phase had decreased hardness values due to its presence in the alloy. Therefore, the JR6 alloy, which presented a large amount of eta phase [17], had a lower hardness than the JR5 alloy. The ANOVA of the hardness results are shown in Table 3, where the P-value (which is lower than 0.05) confirms that the impact of the alloying elements on the hardness was statistically significant.

Table 3.

Analysis of variance (ANOVA) of the alloy composition on the hardness.

Parameter  DF  SS  MS  P-Value 
Composition  167971  23996  140.79.74E-08
Residuals  1365  171 

On the other hand, the fracture toughness decreased as the hardness increased (Fig. 7). For high R values, there was more free Co which increased the energy required for crack propagation and thus improved the fracture toughness. Nevertheless, due to data dispersion, the ANOVA results of the fracture toughness (Table 4) showed a high P-value, showing that the change in chemical composition on the fracture toughness did not have statistical significance.

Fig. 7.

Hardness to toughness relation of the sintered alloys.

(0.13MB).
Table 4.

ANOVA of the alloy composition on the fracture toughness.

Parameter  DF  SS  MS  P-Value 
Composition  9.63  1.38  2.60.102
Residuals  4.23  0.53 

The wear test results are shown in Fig. 8 where the alloys with R values of 3 and 12 (corresponding to 6 wt%) had the lowest volumetric loss. The hardness was shown to be the main parameter regarding abrasive wear behavior, consistent with other research [21–23]. Alloys that developed the η phase had few zones of detachment between the general abrasive wear, therefore reducing their wear resistance. Alloys with high R values had the lowest wear behavior due to the increased amount of binder phase subjected to abrasive flow by the alumina particles during the test. It was also found that increased amounts of W dissolved in Co, which was influenced by the addition of 0.5 wt% of Cr3C2, did not improve the wear behavior of those alloys. The ANOVA (see Table 5) confirms statistical the significance of the volumetric loss changes

Fig. 8.

Mean volumetric loss of the sintered alloys.

(0.15MB).
Table 5.

Analysis of variance (ANOVA) of the alloy composition on the volumetric loss.

Parameter  DF  SS  MS  P-Value 
Composition  3770  538.6  12.990.00085
Residuals  332  41.5 

Since the ANOVA tests showed significant differences in the hardness and volumetric loss means, a statistical Least Significance Difference “LSD” test was performed to determine which alloys had the best performance. RStudio statistics software was used to make the groups using “Agricolae” library and the “BH” adjustment method to mitigate the false discovery rate. The results of this test can be found in Table 6, where the rigth and left zones represent the differences between means of volumetric loss (mm3) and hardness (HV30) respectively, in the column-row intercept. If a pair of alloys have a difference in means lower than the computed LSD value, the alloys were classified in the same statistical significance group. The groups are listed in alphabetic order where the “a” letter was given to the high significance group, and as seen the only two pairs of alloys with no significant difference in the hardness were JR6 and JR8 which are in the group “e,” and JR5 and JR7, which are in group “c”. The result above confirms that the “R” number was the main factor influencing the hardness, followed by the starting TiC content.

Table 6.

LSD test results of the hardness and volumetric loss.

TiC [wt%]  R [wt%]  Alloy  JR1  JR2  JR3  JR4  JR5  JR6  JR7  JR8  Significance groups , α:0.05
                      Hardness LSD: 30.12 [HV30]  Wear LSD: 14.85 [mm3
JR1  –  37  2.8  14.3  6.5  26.6  9.5  40.3  cd 
4.5  JR2  251.2  –  39.8  22.7  30.5  10.4  27.5  3.3 
JR3  52.4  303.5  –  17.1  9.3  29.4  12.3  43.1 
4.5  JR4  74.3  176.9  126.7  –  7.8  12.2  4.8  26  bc 
12  JR5  32  219.2  84.4  42.3  –  20.1  33.8  cd 
18  JR6  205.3  45.9  257.7  131  173.3  –  17  13.7  ab 
12  JR7  32.9  218.3  85.2  41.5  0.9  172.5  –  30.8  cd 
18  JR8  187.5  63.7  239.8  113.2  155.5  17.9  154.6  – 

The significance groups from the LSD test applied to the wear results showed that four alloys were in group “d”, which performed the best among the samples tested herein, and all of them had a composition of 6 wt% of Co. The lack significant differences in the wear test can be explained by the high dispersion of the data, which indicates that an increased number of samples would be needed to evaluate among them with statistical confidence. Although, the starting TiC content improved the hardness and wear resistance of the alloys, it simultaneously decreased the fracture toughness. Nevertheless, that reduction did not considerably affect the wear behavior of the alloys.

4Conclusions

Eight TiWCrC-Co alloys were sintered in an alumina vacuum furnace, and the microstructural and mechanical characterization allowed us to conclude the following:

Cr3C2 and TiC dissolution contributed free carbon to the alloys, inhibiting the formation of the η phase; thus, the lower the content C of these compounds was, the higher the tendency to develop the η phase. Furthermore, these compounds were shown to be a good additive to the WC-Co alloys due to wear resistance improvements and decreased volumetric cost. Thus, there are potential applications in anti-wear parts that experience very high abrasive conditions; however, due to the apparent decrease in the fracture toughness values, these alloys are not as promising for applications that experience impact.

The wear behavior of the sintered alloys showed a high dependence on the hardness. Increased TiC content showed two positive effects: The formation of the hard TiWC2 phase, was beneficial, and the hindrance of the Ostwald ripening process of the WC phase due to its development throughout the microstructure was benefical, despite the decrease in the fracture toughness. Moreover, an increased Co saturation with Cr inhibited WC grain growth efficiently, without the formation of undesired Cr-rich phases.

Acknowledgments

The authors thank the Powder Metallurgy Laboratory of Universidad Nacional de Colombia Sede Bogota, and the Centro de Materiales y Ensayos of SENA, Regional Distrito Capital, for the logistical, technical, human and financial support of the project. This work was financed with resources from the Patrimonio Autónomo Fondo Nacional de Financiamiento para la Ciencia, la Tecnología y la Innovación, Francisco José de Caldas under the PULFAB Project with contingent recovery contract FP44842-091-2016.

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