Mechanical performance and thermal shock resistance of alumina composites fabricated by temperature gradient spark plasma sintering

DOI: https://doi.org/10.21203/rs.3.rs-44210/v1

Abstract

Temperature gradient spark plasma sintering technology (TGSPS) was used to fabricate alumina composites with addition of tremolite. The mathematics model of TGSPS was established using piecewise interpolation spline function. Liquid phase sintering took place in the sintering process. Vickers hardness, fracture toughness and flexural strength of the composites were measured. Microstructure observations on fracture surfaces of alumina composites were analyzed. Thermal shock resistance of alumina composites was investigated by measuring the strength retention after varying the temperature difference through the water-quench method. Results showed that the addition of tremolite could promote the liquid phases sintering of alumina composites, decrease the porosity, strength the grain boundaries, improve the mechanical properties, and thus contribute to the improvement in TSR of alumina composites.

1. Introduction

Recently, alumina ceramic composites have been receiving growing attention owing to their sound mechanical performances such as high hardness, good chemical inertness, high wear resistance, and so on. High-quality alumina ceramic bodies are widely used for casting hollow turbine blades in aircraft engines and gas turbines [1], ceramic cutting tools for machining hard materials [2, 3], ceramic nozzles in sand blasting treatments[4, 5], Spark plugs[6], coatings[7–9], bearings [10, 11] and dental materials[12]. It is well known that the addition of CaO could cause alumina to crystallize at low temperature and promote the sintering process [13]. Meanwhile, the addition of small amounts of MgO suppresses abnormal grain growth of alumina, induce liquid-phase sintering and promote enhanced densification rate [14–20], so fine microstructures and good mechanical properties of alumina ceramic composites can be obtained if MgO is introduced with appropriate content. It has been reported in reference [21] that, the smaller the sizes of particles are, the lower the temperature to sinter alumina will be. Being composed of SiO2, CaO and MgO phases, tremolite (Ca2Mg5Si8O22(OH)2), which is a member in amphibole groupwhich and can be formed by the conversion of dolomite, silica and water together with calcite and carbon dioxide[22], is expected to decrease the sintering temperature of alumina ceramic materials.

Spark plasma sintering (SPS) has the characteristics of fast rising and cooling, low sintering temperature and short holding time, which can reduce the abnormal growth of particles [23–25]. It is possible to achieve high densification Al2O3 composite prepared by SPS at low temperature, which suppresses its grain growth [26–28]. The densification of Al2O3-YSZ-TiO2 composites sintered by SPS at temperature of 1350–1400 °C was higher than 99.2% [28]. The average grain size of Al2O3/WC composite fabricated by SPS was 1-1.5 µm [29]. The hardness and flexural strength of Al2O3-Ni nano composites fabricated by SPS at 1573 K reached 20.5 GPa and 170 MPa [27]. The effect of grain refining can be achieved with the help of SPS approach. Nano-structured alumina composite was prepared from micro-sized powders sintered by SPS at 1200 and 1300 °C when the starting powder was 3 µm [30].

Thermal shock resistance (TSR) is one of a major topic for the application of alumina composites in the high-temperature environment. The TSR has been investigated by various researchers for better understanding the mechanisms of improving TSR of Al2O3 composites [31–35]. The improved TSR of Al2O3-SiCw composites were achieved by enhancing its densification and the content of yttrium aluminum garner, producing of tabular alumina [31]. The TSR of laminated Al2O3/Mo-Al2O3 composites was improved by introducing heat-resistant particles into weak layers and improving the interfacial bonding strength of the two layers [32]. The effect of different additives on TSR of Al2O3 composites is various, and some additives can decrease the TSR of Al2O3 composites. The TSR of porous Al2O3 composites was enhanced by introducing SiC nano powder, while the TSR of the samples with micro-sized SiO2 was slightly lower than that of unmodified porous Al2O3 ceramics [33]. The TSR of Al2O3 composites was sensitive to quenching treatment, however the loss of strength was gradual when Al2O3-Er3Al5O12 composite was quenched in boiling water [34]. There are many factors influencing the TSR of ceramic composite, including mechanical properties and thermal physical parameters, thermal expansion coefficient, etc.[36]. The TSR of laminated Al2O3 composites could be characterised by the method of macro features (displacement and residual strength) and micro features (crack growth resistance and fracture mode) [35], which provided the comprehensive understanding of the TSR of Al2O3 composites.

Accordingly, much effort has been made to prepare alumina composites using various technologies mentioned from the above, however, so far the effect of tremolite on the thermal shock behavior of alumina composites, fabricated by TGSPS, is very limited. In this paper, TGSPS was used to fabricate the alumina composites. TGSPS was expected to enhance the densification of alumina composites by avoiding heating too fast compared with the traditional SPS technology. The effects of the tremolite on the mechanical properties, microstructures and TSR of the composites were investigated. The results could contribute to developing a new approach to fabricate alumina composites with good TSR and mechanical properties.

2. Experimental Procedure

2.1. Preparation of the composites

α-Al2O3 of high purity (99.9%) and small grain size(0.5 ~ 1 µm), produced by Zibo Lucky Star Ceramic Company, Shandong province, China, was used as the starting material. Tremolite with grain size of 1 ~ 2 µm and composed of SiO2 (59.8 wt.%), CaO (14.7 wt.%) and MgO (25.5 wt.%) was used as the additive. Powders of commercial α-Al2O3 and tremolite were mixed thoroughly in proper mass proportions, as listed in Table 1, and milled with alumina balls for 90–100 h in an alcohol medium to obtain a homogeneous mixture. The ball to powder mass ratio is 3 to 1 and that of alcohol to powder is 2 to 1. The mixture was dried in vacuum and screened. And then placed in a graphite die using the technology of TGSPS at temperature of 1350 ℃ with pressure of 35 MPa for 5 min.

Table 1

Compositions and mechanical properties of TGSPS sintered alumina composites

Sample

Compositions (wt.%)

Relatively density(%)

Vickers hardness (GPa)

Fracture toughness (MPa·m1/2)

Flexural strength (MPa)

PAO

100% Al2O3

98.5

17.6 ± 1.0

4.65 ± 0.2

391.6 ± 15

AOT2

98% 100 + 2% tremolite

98.6

18.3 ± 1.5

4.50 ± 0.3

416.3 ± 12

AOT4

96% 100 + 4% tremolite

99.2

20.1 ± 1.3

4.77 ± 0.4

503.5 ± 18

AOT6

94%100 + 6% tremolite

99.3

18.4 ± 1.1

4.15 ± 0.1

538.2 ± 10

AOT8

92% 100 + 8% tremolite

99.5

17.2 ± 1.4

4.30 ± 0.2

472.5 ± 21

Table 2

TGSPS sintering process (~ 30 min)

Temperature

[℃]

20-

700

700-

1000

1000-

1350

1350

1350-

1000

1000-

50

50

Speed of heating up and cooling [℃/h]

150

80

60

5 min holding

200

110

Open the

furnace

door

2.2. Characterization

Rectangular bar specimens of size 3 × 4 × 36 mm3 were used for mechanical properties and TSR tests, as shown in Fig. 1. The bars were ground with a diamond wheel and polished using diamond pastes to a Ra of ~ 0.1 µm. Three-point-bending was used to measure the flexural strength on an electronic universal experimental instrument (WD-10, produced by Jinan TEST Co., Ltd. P.R. China) with a span of 20 mm at a crosshead speed of 0.5 mm min− 1. Six specimens with the same compositions were used for measuring the flexural strength in air at room temperature.

The flexural strength was calculated by the following formula [37]:

where σf was flexural strength (MPa) and P was load (N) under which the samples broke, b and h were width and height (mm), respectively, and L was span (mm).

Vickers hardness was measured on polished surfaces with a load of 9.8 N for 5 s with a micro-hardness tester (MH-6). Indentation fracture resistance measurement was performed using the indentation method with a hardness tester (Hv-120, produced by Shanghai Hengyi electronic testing instrument corporation, P.R. China), and results were obtained by the formula proposed by Cook and Lawn [38]. Five indents were made in a row at the middle of each specimen to obtain an average value. XRD (D/max-2400) analysis was adopted to identify the phases after sintering. Microstructures of the samples were studied on fracture surfaces by scanning electron microscopy (SEM, HITACHI S-570, produced by Japan Hitachi Co., Ltd.).

Ground and polished rectangular bars for thermal shock testing were placed into a furnace and heated to the desired temperatures at a heating rate of 20 ℃/min. After the specimens were heated for 30 min in the furnace to induce the homogeneous temperature distribution, they were dropped into a bath of water at room temperature. ΔT, the temperature differences for all composites were chosen referring to literature [35, 38–41]. The experiment temperature differences are 200, 300, 400, 500 and 600℃, respectively. The flexural strengths of the specimens after thermal shock at each temperature were also measured by three-point-bending method. The results were the average value of a minimum number of six specimens tested in the same condition. The surface of the specimens after thermal shock examined by the same SEM equipment with that of before thermal shock tests.

3. Results And Discussion

3.1. Mathematics model of temperature gradient spark plasma sintering

The spline interpolation feature points, as listed in Table 3, were obtained according to the given conditions listed in Table 2.

Table 3

The spline interpolation feature points during the sintering process

(t0,T0)=(0,20)

(t1,T1)=(4.5,700)

(t2,T2)=(8.3,1000)

(t3,T3)=(14,1350)

(t4,T4)=(19,1350)

( t5,T5)=(21,1000)
 

( t6,T6)=(30,50)

  

where T represented the sintering temperature and t was the sintering time. The sintering temperature changed evenly as time went in each temperature interval. The functional relation of temperature and time was as follows:

where Ti and Ti+1 represented the sintering temperature at i and i + 1. ti and ti+1 represented the sintering time at i and i + 1. It was indicated that the relationship between sintering temperature and time was a linear interpolating function of subsection splines, and it was a line chart. The sintering temperature was raised or reduced constantly in every temperature interval and the rising of whole temperature was decelerated. It spent approximately 30 min in the whole SPS process, in which 5 min holding time was used.

3.2. X-ray diffraction phase analysis

The X-ray diffraction phase analysis of sample AOT4 is shown in Fig. 2. It was clear that there existed Al2O3, SiO2 and Ca3SiO5 phases in sample AOT4. The following chemical reaction, yielding Ca3SiO5, may occur during the sintering process:

3CaO + SiO2→Ca3SiO5 (3)

The Gibbs free energy, of reaction (3) was − 162KJ at the temperature of 1350℃, which indicated that reaction (3) was possible to take place based on thermodynamic analysis. X-ray diffraction phase analysis of sample AOT4 confirmed reaction (3).

3.3. Mechanical properties

The mechanical properties of TGSPS sintered alumina composites are listed in Table 1. Vickers hardness, fracture toughness and flexural strength of pure alumina (sample PAO) was 17.6 GPa, 4.65 MPa·m1/2 and 391.6 MPa, respectively. Addition of tremolite significantly improved the performances of TGSPS sintered composites, whose Vickers hardness, fracture toughness and flexural strength reached their maximum value of 20.1 GPa, 4.77 MPa·m1/2 and 538.2 MPa, respectively. The hardness and toughness of the composites increased with increasing tremolite content from 2 to 4wt.%, and then decreased from 4 to 8wt.%. There were two factors influencing the hardness of composites, namely a hardness effect due to the addition of tremolite and a densification effect of the composites. In the first stage (2 to 4wt.% addition), the densification effect was dominant and the hardness was enhanced, while the hardness was reduced as the hardness effect was in turn becoming dominant (4 to 8wt.% addition) for the reason that the hardness of tremolite were lower than that of alumina. Fracture toughness increased with increasing the amount of tremolite before 4 wt.%, at which point it reached the maximum value of 4.77 MPa·m1/2, and then decreased after 4 wt.%. Flexural strength reached its maximum value for sample AOT6 with 6 wt.% tremolite addition and then decreased for further tremolite addition. This trend of flexural strength correlated with the microstructures of the composites, which would be discussed in Sect. 3.5.

It was obvious that the TGSPS sintered alumina composites exhibited significant improvement in mechanical properties. Composite with an addition of 4 wt.% tremolite showed excellent mechanical properties, the hardness, fracture toughness and flexural strength of the composite were enhanced by 14.2%, 2.6% and 28.6%, respectively, with respect to sample PAO sintered under the same conditions.

3.4. Thermal shock resistance

Figure 3 shows a plot of residual flexural strengths versus temperature difference (ΔT) for alumina composites after the water-quenching tests. A three-stage behavior of flexural strength, which is co-incidence with the Hasselman’s theory, was presented, and all the samples exhibited a drastic reduction in flexural strength compared with their initial strengths. The residual strength of sample PAO was lower than that of sample AOT4 and AOT6 through the entire range. The curve for sample PAO showed a critical temperature difference (ΔTc) of 320 ℃ and the characteristic sharp loss of flexural strength at the point, followed by a gradual decrease for further increasing. ΔTc of sample AOT4 and AOT6 was 372 and 360 ℃, respectively. Sample of AOT4 and AOT6 showed appreciably greater ΔTc and residual strength after ΔTc than sample PAO. The results demonstrated that the addition of tremolite in alumina modified the composites mechanical properties and, hence improved the thermal shock behaviours.

3.5. Analysis of microstructures

SEM photomicrographs of fracture surface of samples PAO, AOT4 and AOT6 are shown in Fig. 4. The grain boundaries of sample PAO were unobservable and the fracture mode was mainly transgranular. There existed apparent pores (marked with arrow in Fig. 4a) on the fracture surface of sample PAO. Pores in samples AOT4 and AOT6, however, were much fewer than that in sample PAO, which showed that the addition of tremolite decreased the amount of pores in TGSPS sintered alumina composites. The eliminating of porosities contributed to a certain extent enhanced flexural strength of samples AOT4 and AOT6. The sintering temperature was 1350 ℃, which was higher than the melting point of tremolite, liquid phase might appeare in the TGSPS process. The eliminating of porosities might be mainly due to the smooth flowing of liquid phases, which was formed by tremolite. There were some smaller grains formed in the crystal boundaries for sample AOT4 (circled in Fig. 4b). These small particles formed in a typical intergranular fracture mode, extending the path of crack growth, and contributed to the improvement of fracture toughness for sample AOT4. The fracture surfaces of sample AOT6 (Fig. 4c) were relatively rough and presented brittle character. As was previously discussed in Sect. 3.2, during the TGSPS process, interface reaction took place among CaO and SiO2 to yield Ca3SiO5, existed on the crystal boundaries of alumina composites, strengthened the grain boundaries of the composites, and as a result, contributed to the improvement in flexural strength of alumina composites.

The effect of porosity on mechanical properties is as follows: [42, 43]

M p= Mp0 exp (-bVfp) (4)

Where Mp was the mechanical property, Vfp was the volume fraction of porosity, b was an empirical constant and the subscript 0 indicated zero porosity. The following Eq. (5) could be concluded from Eq. (4):

Where R represented the thermal shock parameters, bσ and bE was empirical constant for the flexural strength and Young modulus of alumina composites, respectively. Usually bE < bσ [44–46], so the higher the Vfp is, the lower the R is, and the poorer the TSR of composites will be. There were some pores existed in the fracture surface of sample PAO (Fig. 4a), fewer pores were found in the fracture surfaces of sample AOT4 and AOT6 (Fig. 4b and c), indicating that the improved TSR was obtained for sample AOT4 and AOT6 comparing with sample PAO. It was concluded that the addition of tremolite could promote the liquid phases sintering of alumina composites, decrease the porosity, strength the grain boundaries, improve the mechanical properties, and thus contribute to the improvement in TSR of alumina composites.

Figure 5 indicates the schematic of the mechanisms of interactions between the crack and particles. Comparing Fig. 5a with b, one could find that the difference in the opening displacement of crack tip between different sizes of grains when the crack propagated the interface between different sizes of grains (Fig. 5b), which would result in the fact that the crack propagated along the big grain. This meant that the crack was locally blunted, and the propagation length of the crack was extended, which contributed to the improvement of fracture toughness for sample AOT4.

The fracture surface morphologies of alumina composites at ΔT = 400 °C are presented in Fig. 6. A flat fracture surface was found for sample PAO at ΔT = 400 °C, and the sample remained the transgranular fracture type. The flatter and large size cleavages extended over the entire fracture surfaces, indicating that the cracks propagated fairly easy across sample PAO without crack deflections like Fig. 5a, and the cracks penetrated the alumina particles at ΔT = 400 °C (Fig. 6a) without appreciable resistance, giving rise to great drops in its residual strengths, which could explain the poor TSR of sample PAO. The enhancement of the residual strength of the alumina composites was attributed to the microstructure evolution of composites after thermal shock, and the microstructure of the samples after the quenching test provided an insight on the important details of thermal shock behavior. The fracture surface of sample AOT4 and AOT6 at ΔT = 400 °C (Fig. 6b and c) showed a relatively rough surface with a fracture mode of the combination of intergranular and transgranular failure. Dimple with a characteristic of ductile fracture could be obviously observed in Fig. 6b (marked with arrow), showing the pullout of alumina grains and indicating the high residual flexural strength of sample AOT4 at ΔT = 400 °C. Transgranular cleavage was found in the fracture surface of sample AOT6 (marked with arrow in Fig. 6c), indicating a relative lower residual flexural strength of sample AOT6 than that of AOT4.

The alumina composites were sintered to a high densification rate (Table 1) and there remained few pores in alumina composite, which enhanced the resistance to the crack initiation and load-bearing capacity of alumina composites. The compact structure of alumina composites led to a better flexural strength of alumina composite. Sample AOT6 has the higher initial flexural strength (538.2 MPa) than sample AOT4 (503.5 MPa), According to the theory of thermal shock fracture, sample AOT6 was more resistant to crack initiation. However, its ΔTc was lower than that of sample AOT4. Sample AOT4 has the higher initial fracture toughness (4.77 MPa·m1/2) than sample AOT6 (4.15 MPa·m1/2), which meant sample AOT4 possessed higher resistance to crack propagation. It was confirmed that the crack propagation rather than crack initiation dominated TSR in current composite ceramic system. It is well known that the flexural strength and fracture toughness are the most important factors to influence the TSR of ceramics [47–50]. The TSR of composites could be assessed by using the critical crack length, Lc, as follows [49]:

where KIC was the fracture toughness of the composites. The improvement of LC contributed to the enhanced TSR of alumina composites. Sample AOT4 had the higher LC value (0.014) than that of sample AOT6 (0.01), which could explain the improvement in the TSR of sample AOT4.

4. Conclusion

Alumina composites were fabricated by TGSPS technology. The mathematics model of TGSPS was established using piecewise interpolation spline function. The following conclusions were obtained:

  1. The relationship between sintering temperature and time was a linear interpolating function of subsection splines.
  2. Composite with an addition of 4 wt.% tremolite showed excellent mechanical properties, the Vickers hardness, fracture toughness and flexural strength of the composite were 20.1 GPa, 4.77 MPa·m1/2 and 503.5 MPa, respectively.
  3. Liquid phase sintering occurred in the TGSPS process, the smooth flowing of liquid phases contributed to the eliminating of porosities, which led to improved mechanical properties of the alumina composites.
  4. The improved TSR was attributed to increased fracture toughness by moderate tremolite addition and the eliminating of porosity

Declarations

Acknowledgements

The authors are grateful for financial support from the National Natural Science Foundation of China (Grant Nos. 51505208), Key Technology Research and Development Program of Shandong province (Grant No. 2019GGX104085), Natural Science Fund project in Shandong province (Grant No. ZR2018PEE010) and Scientific Research Projects in University of Shandong province (Grant No. J18KA031).

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