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Abstract

To improve the adaptability to complex shaped products, TiC particulates (TiCp) reinforced high-manganese steel matrix (TiCp/HMS) composites were prepared by the squeeze casting infiltration method, and the microstructure and the mechanical properties of the composites were investigated, with different TiCp volume fractions (35%, 50%, 65%). Water glass was applied as binder in the TiCp preforms, in which iron powder was added to adjust the TiCp fractions, and Si powder to activate the bonding of TiCp/steel interface. The results showed that with the increase of the volume fraction, the hardness of the composites increases gradually, with the highest reaching 60.7 HRC at 65 % TiCp, which is 2.7 times that of the matrix. However, the bending strength decreases gradually, with the maximum 439.0 MPa obtained at 35% TiCp. The impact toughness of the composites changes slightly. Due to the use of water glass, brittle glass phase is formed at the TiCp/steel interface, which reduces the mechanical properties of the composites. The addition of Si powder can improve the comprehensive mechanical properties of the composites.

Keywords

pressure infiltration TiC particles steel matrix composites bending strength impact toughness

Introduction

Ceramic particles reinforced iron matrix composites combines the high strength and toughness of the steel matrix with the unique advantages of high hardness and high wear resistance of the ceramic particles, and has become one of the hot spots in the field of wear-resistant materials at home and abroad in recent years.¹ At present, in the ceramic particles reinforced iron matrix composites, the commonly used reinforced ceramic particles are TiC, WC, Al₂O₃, SiC, etc.² Among them, titanium carbide (TiC), due to its superior mechanical properties (hardness, modulus and wear resistance), good wettability with iron matrix and wide application in mining, cement, metallurgy, agricultural machinery, and other fields,^3,4 is especially suitable to be selected as reinforcement,^5–7 which has attracted more and more attention.^8–13 Taking the cermet-embedded hammer as an example, the high-manganese steel with excellent toughness is used as the hammer body and the matrix of the cermet (composites), and TiCp reinforced high-manganese steel matrix composite (TiCp/high-manganese steel, TiCp/HMS) as the cermet of the striking surface to improve the wear resistance of the hammer, especially under impact conditions.

Typically, TiCp/steel composites are fabricated using traditional powder metallurgy (PM) methods.¹⁴ Z. Wang et al.¹⁵ reported that TiCp (>60 % by volume) enhanced the microstructure and mechanical properties of 35CrMo steel composite by vacuum sintering process, and its hardness was 65HRC. Shoufa Liu et al.¹⁶ prepared TiC/316L stainless steel composite by PM method. They studied the microstructure, density, hardness, and bending strength of TiCp/316L steel composite, with the TiCp increase from 30 wt% to 90 wt%, and found that the hardness of the composite gradually increased with the increase of TiCp. When the addition of TiCp is 80 wt%, the density of the composite is 99.1%, the hardness is 88.9HRA, and the bending strength reached 1373 MPa.

Although the composites prepared by PM have uniform microstructure and good mechanical properties, there are still some shortcomings. For example, only products with simple appearance can be prepared, and then they need to be fixed to large or complex wear-resistant products through connection processes such as brazing, which has the problem of low connection strength and is prone to fracture and falling off during application.¹⁷ This will not only cause large economic losses, but also affect the production schedule,^14–16 affecting the promotion and application of wear-resistant composites in engineering.

In the early stage, the project team carried out a lot of research work on the preparation of Al₂O₃p reinforced steel matrix composites and various architectured composites by squeeze casting infiltration (casting infiltration) technology.¹⁸ These work shows that, compared with PM, squeeze casting infiltration method achieves the integration of the preparation of composites and the overall forming of the wear-resistant products, so there is no need for the secondary connection, which can be applied to various complex shapes of wear-resistant products, and the interface of composites and wear-resistant products is firmly combined, and the composites are not easy to fall off in service.

In order to overcome the shortcomings of traditional powder metallurgy methods to prepare composite materials, this research group proposed to prepare titanium carbide reinforced high-manganese steel base (TiCp/HMS) composite materials by extrusion and die casting infiltration process and studied the effects of different volume fractions on the microstructure and properties of TiCp/HMS composites. The relationship between microstructure and mechanical properties of TiCp/steel composites under the new process was investigated, which provided guidance for the preparation of high strength and high toughness TiCp/steel composites.

Specimen preparation and test method

Specimen preparation

The chemical composition of the matrix steel (ZGMn13-4 high-manganese steel) is 1.4% C, 10% Mn, 2.0% Cr, 0.4% Si, <0.05% S, and <0.1% p, with the remained Fe. As the reinforcement, TiCp with 99.9% purity (produced by Qinghe YuanYao Alloy Products Co., Ltd) with an average size of 1250 mesh was used, and the TiCp exhibited irregular shapes, as shown in Figure 1(a). The TiCp preforms were made by a uniaxial pressing of 20 MPa with a rectangular mold sized 55 mm × 25 mm × 15 mm, and the microscopic morphologies of the preforms are shown in Figure 1(b). The preforms were subsequently sintered at 500°C for 2 h under vacuum conditions. During the casting infiltration, a preform was first fixed inside a steel die, which was cated inside with an insulating ceramic tube with an inner diameter of 90 mm; then, the molten metal liquid was pouring into the die, followed by squeeze casting. The squeeze casting parameters include a pressure of 50 tons, the pouring temperature of 1600°C, and a holding time of 15 s.

Figure 1.

Micromorphologies of raw and preformed TiC powder. (a) Raw material TiC powder (b) TiC preforms after sintering.

Microstructure characterization

The microstructures and fracture morphologies of TiC powder, preforms and composites were observed by scanning electron microscopy (SEM, LEO-1450). The volume fractions of the composites were measured from five SEM images using the Image-Pro Plus analysis program. The crystalline phases in the matrix alloy and the composites were characterized using X-rays (XRD; D MAX-2500, Science) with Cu Ka1 as the monochromator, and its specific parameters included a scanning speed of 2°/min and a scanning range of 2θ = 10°∼100°. The obtained XRD data were processed and analyzed using MDI-Jade 6.5 software. The interfacial morphologies and elements were characterized using TEM (JEM200). The elemental distributions of the matrix alloys and the composites were checked using electron probe microanalysis (EDS; Oxford Xplore 30).

Characterization of mechanical properties

The hardness of the materials was tested with a Rockwell hardness machine according to Chinese standard GB/T230.1-2004. The measured surface of the specimen must be polished with 80 mesh to 1000 mesh sandpaper to ensure that the measured surface was parallel to the bottom surface. To avoid large fluctuations in the hardness tester readings, affecting the accuracy of the experiment, a multipoint measurement was used to take the average to determine the final hardness value. The bending strength test was conducted according to Chinese standard GB/T3851-2015. The rectangular specimens for the test had a size of 5 mm × 5 mm × 30 mm. The specimens were first cut with a wire cutting machine. Then the four test surfaces of the specimens underwent sandpaper grinding. The impact toughness test was carried out on a Charpy impact machine according to the Chinese standard GB/T9096-2005, and the impact toughness specimens were rectangular and sized 10 mm × 10 mm × 50 mm without notch. The data provided above were the average of three measured values.

Results and discussion

Microstructure

The microstructure of the TiCp/steel composites is shown in Figure 2 (a) and (b). TiCps are uniformly distributed in the matrix, with an area fraction of approximately 50% (±2%); this value is the same as that in the preforms. From Figure 1(a), no burnout occurs at the boundary of TiCp, which differs from the raw powder.^19,20 There are dark streaks and white rounded substances at the interfaces of TiCp, which indicates that the binder water glass (Na₂O·3.3SiO₂) in the preforms generates a glass phase at high temperatures during the squeeze casting; thus, the substance is a Ti contained oxide glass phase material. The interface between the matrix and the reinforcing material is clean and free of defects, such as pores, cracks, or debonding. In addition, the infiltration of the steel melt into the preforms can be achieved, even at distances of less than 10 μm between the TiC particles; this finding indicates that TiC has good wettability to the steel melt in the squeeze casting process.

Figure 2.

Microstructure of TiC/high-manganese steel composite manufactured by squeeze casting. (a) Microscopic morphology at 10 μm (b) Microscopic morphology at 2 μm.

The distribution of elements in the matrix and composite was characterized by EDS, and the results are shown in Figure 3. The microstructure in Figure 3 shows that there are dark striped substances and white round substances in the interfaces of TiCp. An energy spectrum comparison shows that the dark striped substances may consist of Si, O, Ti and other elements, and the white round substances contain Fe elements; black substances can be seen near the dark striped substances. According to a comparison of the energy spectra, the black substances are found to potentially consist of Si, O, and other elements. To further determine the phase of the above substances, EDS point scan analysis is performed. First, EDS point scanning is performed on the dark material of the strip, and the elemental composition of the strip can be seen by spectrum a in Figure 4, which is mainly composed of Ti, O, and Si, with trace amounts of Fe and C. O in the substance comes from the binder water glass in the preforms. The water glass generates a glass phase at high temperatures; thus, the substance has a glass phase that contains Ti oxide. The white dots in the figure are analyzed by EDS point detecting, and the main element is Fe, as seen from spectrum b in Figure 3, which may appear due to the iron powder of the preforms not being completely melted by the high-manganese steel melt during squeeze casting. Finally, the black substance near the dark bar is analyzed by EDS point detecting. EDS point scanning analysis of the substance near the dark bar, through spectrum c in Figure 3, shows that its elemental composition mainly contains O, Si, Fe, Ti, and other elements; thus, the substance should be a glass phase containing Fe, Ti, and other oxides.

Figure 3.

EDS surface scan results of the 50% volume fraction TiCp/high-manganese steel composite.

Figure 4.

EDS point scan results of 50% volume fraction TiCp/high-manganese steel composite.

Phase analysis of composite materials

Figure 5 shows the XRD patterns of TiCp/HMS composites with different TiCp volume fractions. The composites are all mainly composed of TiCp and the steel matrix. The peak angles of the characteristic peaks of the composites with TiCp volume fractions of 35% and 50% are basically the same, and the phases are TiCp and α-bcc iron (martensite). When the volume fraction of TiCp increases to 65%, the characteristic peak of martensite disappears, and austenite appears. This phenomenon occurs because during squeeze casting, when the steel infiltrates into the interior of the preforms, the iron powder in the preforms is first melted by the steel melt and then melted into the high-manganese steel; thus, the original Mn and C elements in the steel are reduced, changing the organization of the Mn and C elements.^21,22 When the volume fraction of TiCps is low, the amount of iron powder contained in the preforms is high. XRD results show that the TiCp/HMS composites have been prepared successfully without excess Mn and C elements. Composites are prepared successfully without excess reactive phases and impurities.

Figure 5.

XRD profiles of TiCp/manganese steel composites with different volume fractions.

Mechanical properties

The results of the mechanical property tests of the matrix steel and the composite are summarized in Table 1. The hardness of the composites increases gradually with the increase of the TiCp volume fraction. The hardness of the composite containing 65% TiCp was 60.7 HRC, which was the maximum, and 167% higher than that of the high Mn steel matrix (22.7 HRC). The hardnesses of the composites prepared with a volume fraction of 21% TiC-reinforced steel were approximately 720 HV and 830 HV.²³ The hardness of the 70 vol% TiC-reinforced stainless steel produced by the powder technique was approximately 1035 HV.²⁴ Therefore, the hardnesses of TiC-high-manganese steel composites produced by any process increased with increasing titanium carbide amount, with an effective transfer from soft to hard reinforcement. According to the bending test results, the bending strength of the composites decreases gradually as the volume fraction of TiCp increased. The highest bending strength is 439.0 MPa at 35% TiCp, which is 65.9% lower than that of the high-manganese steel matrix (1288.3 MPa). According to the impact toughness test results, the impact toughness of high Mn steel matrix is 223.2 J/cm²; however, the impact toughness of the composites was much lower, which are 2.4 J/cm², 2.3 J/cm², and 2.5 J/cm² for the composite specimens with volume fractions of 35%, 50%, and 65%, respectively. So, the impact toughness of the composites at different volume fractions did not change much. Compared with the matrix, the composites exhibited poor bending strength and impact toughness levels. This phenomenon occurred mainly due to the presence of a black layer of a glassy phase material at the interfaces between the TiCp and the steel matrix, which significantly decreases the bending strength and impact toughness values of the composites with respect to the steel matrix.

Table 1.

Mechanical properties of different volume fractions of TiCp/manganese steel composites.

Specimen number	Volume fraction (%)	Hardness (HRC)	Bending strength (MPa)	Impact toughness (J/cm²)
W0	0	22.7	1288.3^a	223.2
M1	35	52.9	439.0	2.4
M2	50	57.0	401.4	2.3
M3	65	60.7	151.3	2.5

^aThis value is not final because the sample was not broken due to the safety of the test equipment.

Figure 6 shows the engineering stress–strain curves of the composites at different volume fractions and the steel matrix specimens during the bending strength test. Figure 6 shows that the overall trend of the engineering stress-strain curves of the composites at different volume fractions is basically the same as that of the matrix material; that is, the bending strength of each specimen increases continuously with increasing engineering strain during the bending test. According to the curves in Figure 6, the bending strength of the high-manganese steel matrix is significantly better than that of all composites. The engineering stress–strain curves of the composite specimens with different volume fractions show that the bending strengths of those with 35% volume fraction are the largest, and the bending strengths of those with 50% volume fraction are similar. The bending strengths of the 50% volume fraction composite specimens have the largest increases in bending strength; thus, there is room for further improvement in the flexural resistance of 50% volume fraction composite specimens.^25,26

Figure 6.

Bending stress–strain curves of different volume fraction composites and the high-manganese steel matrix.

Figure 7 shows the impact load–displacement curves of the composite and high-manganese steel matrix with different volume fractions during the impact toughness test. In Figure 7, the general trend shows that the maximum impact loads of the specimens with different volume fractions of TiCp gradually decrease as the volume fraction of TiCp increases, the area of the impact load–strain curve does not change much, and the impact toughness values of the TiCp/high-manganese steel composites do not change much with the increase in the volume fraction of TiCp.

Figure 7.

Impact load-displacement curve of different volume fractions of TiCp/high-manganese steel composite materials and the high-manganese steel matrix.

Fracture analysis

Figure 8 shows the fracture microscopic morphologies of the bending strength specimens with different volume fractions. Figure 8(a) shows the fracture morphology of the high-manganese steel matrix specimen. The fracture is deconstructed in an obviously river flower-like manner with many tough nests; thus, the toughness of the high-manganese steel matrix specimen W0 is better, and its fracture mode is toughness fracture. Figure 8(b) shows the fracture morphology of a 35% volume fraction composite; the dark gray particles in the fracture are TiCp, and the off-white color represents the high-manganese steel matrix. On the surface of the fracture, there are many brittle fracture planes of TiCp, and there is a dark glassy phase material at the interfaces between TiCp and the steel matrix; some of these fracture planes are marked in Figure 8(b), and the fracture mode is brittle fracture. In Figure 8(c), for the fracture morphologies of 50% volume fraction composites, due to the increase in TiCp volume, the steel matrix organization in the fracture gradually decreases, and the fracture surface of TiCp is a smooth plane after brittle fracture. There is dark glassy material at the interface of TiCp. Figure 8(d) shows the fracture morphology of 65% volume fraction composite, and the white steel matrix microstructure in the fracture decreases in proportion. The bonding effect of the steel matrix is weakened, and the TiCp on the fracture surface is a smooth plane after brittle fracture. In the interface between the TiCp and the steel matrix, there is black glass phase material and white, spherical, reduced-iron powder that has not been melted by the steel.

Figure 8.

Break morphology of the bending strengths of TiCp/high-manganese steel composite materials with different volume fractions. (a) Matrix (b) 35%. (c) 50% (d) 65%.

The bending strength of the composite specimen is lower than that of the high-manganese steel matrix, and it decreases with the increase in TiCp volume fraction, because there are glass phase substances in the microstructure of the composites and because the steel matrix in the microstructure of the composites gradually decreases with the increase in TiCp volume fraction; the bonding effect is gradually reduced, thus the bending strengths of the composite specimens gradually decrease.

Figure 9 shows the microscopic morphologies of the fractured impact toughness specimens of the composites with different volume fractions. In Figure 9, the steel matrices in the fractured impact toughness specimens with different composite volume fractions decrease as the volume fraction of TiCp increases. Figure 9(a) shows the impact fracture morphology of the high Mn steel matrix, and the fracture has obvious destructive steps and many tough nests; this finding indicates that the high Mn steel matrix specimens are very tough and their fracture mode is tough fracture. Figure 9(b) presents the impact fracture morphology of a 35% volume fraction composite. From Fig. (b), the dark gray TiCp and the off-white high Mn steel matrix are obvious. In Fig. (b), the fracture surface of TiCp is smooth and flat, and there is dark glassy phase material at the interface of TiCp; part of the glassy phase material is marked in Figure 8(b). Figure 9(c) shows the impact fracture morphology of a 50% volume fraction composite. The steps of TiCp decoupling fracture can be seen in the high-magnification image of the fracture morphology; the dark glassy phase material is present at the interface of TiCp. Figure 9(d) shows the impact fracture morphology of 65% volume fraction composites, and the dark glassy phase material is present at the interface of TiCp.

Figure 9.

Break morphology of the impact toughness sample of the TiCp/high-manganese steel composite material with different volume fractions. (a) Matrix (b) 35%. (c) 50% (d) 65%.

By combining the impact toughness test results of composites with different volume fractions and based on the findings of the fracture morphology analysis, the following results can be obtained. The impact toughness of the composites is much lower than that of the high-manganese steel matrix, and the impact toughness between composites with different volume fractions decreases with the increase of TiCp volume fraction, the fracture modes of composite specimens with different volume fractions are all basically brittle fracture. Glass phase material can be found in the organization of the various fracture morphologies of the composite specimens with different volume fractions, and the toughnesses of the composites is reduced due to the brittleness of the glass phase material.

Activated micropowder technology

As shown in Figure 10, the microstructures of the composites with different Si powder additions all consist of dark TiCp and an off-white steel matrix; however, with increasing Si powder addition, the black material at the interfaces between the TiCp and the steel matrix gradually increase. The results of the EDS surface scan of the TiCp/Mn13 composite with 3.5 wt% Si powder addition are shown in Figure 11. By comparing the analysis results of the energy spectrum, the black substance at the interfaces between the TiCp and the Mn13 matrix may contain O, Si, Ti, and other elements; the substance should be a glass phase substance containing Ti oxide. The results of the energy spectrum of Si elements in Figure 11 show that Si elements are mainly distributed in the glass phase material around the Mn13 matrix and TiCP; Si elements dissolved into the Mn13 matrix can form solid solution strengthening. This phenomenon occurs because the solid solution of Si in the steel matrix causes large lattice distortion in the ferrite and austenite cells, which leads to solid solution strengthening and increases the hardness of the composite material. The mechanical properties of TiCp / Mn13 composites with different amounts of Si powder are shown in Table 2.

Figure 10.

Microstructures of TiCp/Mn13 composites with different amounts of Si powder. (a) 0 wt.%. (b) 3.5 wt.%. (c) 7.5 wt.%.

Figure 11.

EDS surface scan results of the TiCp/Mn13 composite with 3.5 wt% Si powder.

Table 2.

Mechanical properties of TiCp/Mn13 composites with different amounts of Si powder.

Specimen number	Si powder addition (wt.%)	Hardness (HRC)	Bending strength (MPa)	Impact toughness (J/cm²)
D0	0	53.6	277.4	2.4
D1	3.5	54.9	347.0	2.3
D2	7.5	57.0	401.4	2.3

Figure 12 shows the fracture micromorphologies of the bending strength specimens with different Si powder additions. The results of the EDS surface scan analysis of the fracture micromorphology of the bending strength specimen are shown in Figure 12, displaying the glassy phase material in the fracture microstructure; these glassy phase materials are at the interfaces of the TiCp, and some of the glassy phase materials are marked in Figure 12. Further observation shows the cracks in the fracture microstructure, and these cracks are all along the TiCp and the steel matrix. These cracks are extended along the glassy material at the interfaces between the TiCp and the steel matrix. The impact toughness values of the composite specimens do not change much with increasing Si powder additions because the glass phase material exists at the interfaces between the TiCp and steel matrix in different specimens. The glass phase material is brittle and should fracture first; thus, the crack propagates along the glass phase material. Compared with the solid solution strengthening effect of Si, the glass phase material at the interface has a greater effect on the impact toughness of the composite material.

Figure 12.

Fracture morphologies of the TiCp/Mn13 composites with different amounts of Si powder. (a) 3.5 wt.% (b) 7.5 wt.%.

Discussion

It is found that in the high temperature liquid prepared by the composite material, some atoms of the matrix steel liquid and the atoms of TiC diffuse to the water glass liquid in the preform, and the complex chemical reaction occurs. The formation is very complex and contains some low-density substances and amorphous. It is easy to escape from the composite zone in the liquid, and the formation left after solidification. Combined with the analysis of the literature,²⁷ the reactive interface layer in the composite material contains the amorphous phase Na₂SiO₃. This amorphous phase usually affects the wettability of TiC and molten steel, resulting in poor interfacial bonding. In the future, organic binders (such as PVA) can be tried to be sintered at high temperature to eliminate such defects.

GAO et al found that the bicontinuous TiC/Fe composites were prepared by pressureless infiltration process, and the maximum bending strength was 481 MPa.²⁸ However, the bending strength of the composites in this work was reduced by 40 MPa. Compared with the composite prepared by PM,²⁹ the hardness and impact toughness are not much different, but the flexural strength is reduced by 66%. Although this process has the advantage of high adaptability to complex shape composite, high efficiency, compared with PM, there is a reaction layer of glassy materials at TiCp/steel interface, which affects the wettability of titanium carbide in molten iron and leads to the decrease of material properties. Therefore, the properties of the composites can be further improved by remove of the glassy reaction interface layer.

Conclusions

TiCp-reinforced high Mn steel composites with different volume fractions were prepared by the squeeze casting process, and the effects of volume fractions of TiCp and Si powder addition on the hardness, bending strength, and impact toughness characteristics of the composites were investigated.

(1) The hardnesses of the composites gradually increase with increasing TiCp volume fraction, and the maximum hardnesses reach 60.7 HRC when the volume fraction is 65%.

(2) The bending strength and impact toughness of the composites decreases with increasing TiCp volume fraction; the composite with 50% TiCp composes best comprehensive mechanical properties than the other composites.

(3) The microstructure of TiCp/Mn13 composites with different Si powder addition have relatively uniform TiCp distributions; and the hardnesses tends to increase with the increase of Si powder addition, with the maximum reaching 57.0 HRC, as well as the bending strength reaching the maximum of 401.4 MPa, when the Si powder addition is 7.5 wt%.

(4) The presence of glassy phase material (Na₂SiO₃) at TiCp/steel interface is attributed to the decrease of the strength and toughness of the composites.

Footnotes

Acknowledgments

The authors sincerely acknowledge financial support from the National Natural Science Foundation of China (52261030) and the Major Science and Technology Projects in Yunnan Province (202201AS070026).

Author contributions

Shengnian Zhao: Writing – original draft, Methodology, Investigation, Data curation, Writing – review & editing. Dehong Lu: Project administration, Funding acquisition, Conceptualization, Methodology, Supervision. Fenbing Wang: Investigation, Formal analysis, Writing – review & editing. Jianming Du: Writing – review & editing, Visualization. Jiang Yehua: Supervision, Project administration.

Declaration of conflicting interests

The author(s) declared no potential conflicts of interest with respect to the research, authorship, and/or publication of this article.

Funding

The author(s) disclosed receipt of the following financial support for the research, authorship, and/or publication of this article: This work was supported by the National Natural Science Foundation of China (52261030) and the Major Science and Technology Projects in Yunnan Province (202201AS070026).

ORCID iD

De-Hong Lu

Data availability statement

The data already used is not confidential. All data included in this study are available upon request by contact with the corresponding author.

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Effects of the volume fraction on the microstructural and mechanical properties of TiCp/high-manganese steel composites

Abstract

Keywords

Introduction

Specimen preparation and test method

Specimen preparation

Microstructure characterization

Characterization of mechanical properties

Results and discussion

Microstructure

Phase analysis of composite materials

Mechanical properties

Fracture analysis

Activated micropowder technology

Discussion

Conclusions

Footnotes

Acknowledgments

Author contributions

Declaration of conflicting interests

Funding

ORCID iD

Data availability statement

References