Influence of Alumina (Al2O3) and Titanium Diboride (TiB2) Nanoparticulates on the Microstructure and Properties of Al-Si9-Cu3-Fe1 Alloys for High Pressure Die Casting Applications

This introductory paper is the research content of the paper "Influence of Alumina (Al2O3) and Titanium Diboride (TiB2) nanoparticulates on the microstructure and properties of Al Si9 Cu3 Fe1 alloys for high pressure die casting applications" published by Université Bordeaux I.

Fig. 3.10.: Test procedure
Fig. 3.10.: Test procedure

1. Overview:

  • Title: Influence of Alumina (Al2O3) and Titanium Diboride (TiB2) nanoparticulates on the microstructure and properties of Al Si9 Cu3 Fe1 alloys for high pressure die casting applications.
  • Author: Iban Vicario Gomez
  • Publication Year: 2011
  • Published Journal/Society: Université Bordeaux I (PhD Thesis)
  • Keywords: Al-Si9-Cu3-Fe1, Al2O3, TiB2, nanoparticles, microstructure, mechanical properties, thermal properties, high pressure die casting (HPDC), grain refinement, reinforcement.

2. Abstract

The main objective of the work is to study the influence of TiB2 and Al2O3 nano particles (up to 1 wt. %) on the properties and physical features of aluminium casting alloys processed through an under pressure process known as high pressure die casting. [Page 3]

3. Research Background:

Background of the research topic:

  • High pressure die casting (HPDC) is a widely used process for producing light alloy components, especially in the automotive, transport, and energy sectors. [Page 2]
  • Aluminium alloys are commonly used in HPDC due to their excellent properties and lightweight construction. [Page 2]
  • The Al-Si9-Cu3-Fe1 alloy is the most common alloy used in HPDC. [Page 2]

Status of previous research:

  • Previous research has focused on improving aluminium alloy properties through alloying elements and the use of grain refiners (e.g., Al-Ti-B master alloys). [Page 7]
  • Metal matrix composites (MMCs) have been investigated to enhance mechanical properties. [Page 8]
  • Nanoparticles are being investigated for various applications, including structural applications in light metals. [Page 8]

Need for research:

  • There is a need to develop aluminium cast parts with better mechanical properties at higher temperatures and higher service pressures, while reducing weight. [Page 2]
  • There is limited industrial employment of nanoparticles as refining and reinforcement agents in Al-Si9-Cu3-Fe1 alloys. [Page 2]
  • Specific grain refiners for Al-Si9-Cu3-Fe1 alloys are lacking. [Page 2]

4. Research purpose and research question:

Research purpose:

  • To study the influence of TiB2 and Al2O3 nanoparticles (up to 1 wt.%) on the properties of Al-Si9-Cu3-Fe1 alloys processed by HPDC. [Page 3]

Core research:

  • Analysis of the influence of TiB2 and Al2O3 nanoparticles on the solidification and microstructure of the Al-Si9-Cu3-Fe1 alloy. [Page 3]
  • Analysis of the influence of Al2O3 and TiB2 nanoparticles on the mechanical and thermal properties of the Al-Si9-Cu3-Fe1 alloy. [Page 5]

5. Research methodology

  • Research Design: Experimental study.
  • Materials:
    • Base alloy: Al-Si9-Cu3-Fe1. [Page 3]
    • Reinforcement nanoparticles: TiB2 (commercial and SHS-produced, ~200 nm and mesh 325) and Al2O3 (15-40 nm). [Page 2]
  • Data Collection:
    • Differential Thermal Analysis (DTA) for solidification curves. [Page 3]
    • Optical Microscopy (OM), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), and Atomic Force Microscopy (AFM) for microstructural analysis. [Page 5]
    • Image analysis and elemental analysis (EDS, WDS) to study the influence of nanoparticles. [Page 5]
    • Tensile tests at room temperature and 200°C. [Page 5]
    • Thermal conductivity measurements. [Page 5]
    • Grain Refining test of Aluminium Association (TP1). [Page 9]
  • Analysis Method: Comparison of solidification curves, microstructural features, mechanical properties, and thermal properties between reinforced and unreinforced alloys. Comparison with existing models for calculating mechanical and thermal properties. [Page 5]
  • Sample Preparation:
    Samples of two different reinforcement nanoparticles (Al2O3 and TiB2) has been made in a high pressure die casting machine. [Page 2]

6. Key research results:

Key research results and presented data analysis:

  • TiB2 and Al2O3 nanoparticles influence the solidification behavior of the Al-Si9-Cu3-Fe1 alloy, acting as grain refiners and modifying the microstructure. [Page 122]
  • The addition of nanoparticles generally increases the nucleation temperature and decreases the undercooling. [Page 71]
  • TiB2 particles have a more pronounced effect on grain refinement than Al2O3 particles. [Page 82]
  • Nanoparticles reduce porosity size and quantity. [Page 123]
  • The microstructure of the reinforced alloys shows finer dendrite arm spacing (SDAS) and a more refined eutectic structure. [Page 93]
  • The mechanical properties (UTS, elongation) are generally improved with the addition of nanoparticles, especially TiB2. [Page 129]
  • Electrical conductivity decreases with the addition of nanoparticles. [Page 117]
Figure 4.1.- T=f(t) curve aspects and key parameters in nucleating zone.
Figure 4.1.- T=f(t) curve aspects and key parameters in nucleating zone.
Figure 4.33.- A and B : TEM micrograph of typical microstructure of sample in the center of the foundry sample namely acicular grain zone. Each TEM micrograph (bright field image is associated with 4 EDS corresponding maps (Al, Cu, Si and Fe)).
Figure 4.33.- A and B : TEM micrograph of typical microstructure of sample in the center of the foundry sample namely acicular grain zone. Each TEM micrograph (bright field image is associated with 4 EDS corresponding maps (Al, Cu, Si and Fe)).
Figure 5.9: Fracture analysis of 0.1% Al2O3 gamma alumina reinforced alloy
Figure 5.9: Fracture analysis of 0.1% Al2O3 gamma alumina reinforced alloy
Table 5.3: Comparison of properties obtained with NADCA formula and experimental essays [Mak 98]
Table 5.3: Comparison of properties obtained with NADCA formula and experimental essays [Mak 98]

List of figure names:

  • Fig.2.1: Illustration of cold chamber high pressure die casting. [Page 10]
  • Fig.2.2: Blistering process with entrapped gas porosity. [Page 12]
  • Fig.2.3. (a) and Fig.2.3. (b): Solidification diagrams of Temperature / Time [Ask 03]. [Page 16]
  • Fig.2.4: Determination of critical radius [Ask 03]. [Page 17]
  • Fig.2.5: Undercooling variation between homogeneous and heterogeneous nucleation. [Page 18]
  • Fig.2.6.: Necessary undercooling in function of particle diameter [Que 04-02]. [Page 21]
  • Fig.2.7: AMC processing routes [Mor 01]. [Page 22]
  • Fig.2.8: Reinforcement shape classification of AMC [Mor 01]. [Page 24]
  • Fig.2.9.: Materials employed in MMCs by number of companies [Mor 01]. [Page 25]
  • Fig.2.10.: Stress – strain diagram. [Page 32]
  • Fig.2.11.: Scheme of the crystal structure of TiB2. [Page 36]
  • Fig.2.12.: Scheme of the crystal structure of Al2O3 [Wik 11]. [Page 39]
  • Fig.2.13.: Relation between grain size and hardness [Sch 01]. [Page 44]
  • Figures 3.3: SEM images of TiB2 obtained by SHS with reactor. [Page 55]
  • Figures 3.4: Particle size distribution of TiB2 obtained by SHS with reactor. [Page 55]
  • Figures 3.5: SEM images of SHS milled materials. [Page 56]
  • Figures 3.6.: SEM images of commercial milled materials. [Page 56]
  • Figures 3.7.: SEM images of Nano commercial TiB2 milled with aluminium. [Page 57]
  • Fig. 3.8: Al-Si phase diagram [Zol 07]. [Page 58]
  • Fig. 3.9: Fe phases determination. [Page 58]
  • Fig. 3.10.: Test procedure. [Page 64]
  • Figure 3.11.- HPDC Test bars. [Page 65]
  • Figure 3.12.- Commercial sand cup for DTA determination. [Page 67]
  • Figure 4.1.- T=f(t) curve aspects and key parameters in nucleating zone. [Page 71]
  • Figure 4.2.- Nucleation (Area 1) and Modification (Area 2) curves and arrests. [Page 72]
  • Figure 4.3.- T=f(t) and dT/dt curves with main identified reactions. [Page 73]
  • Figure 4.4.- T=f(t) and dT/dt curves with main identified reactions. [Page 74]
  • Figure 4.5.- Nucleation temperature (Tn) and time (tn) determination. [Page 74]
  • Figure 4.6.- Point of start of liquidus (N) determination with 5th derivative. [Page 75]
  • Figure 4.7.- Eutectic reaction characteristic parameters. [Page 75]
  • Figures 4.8. A and B- Determination of liquidus temperature and precipitations with Thermo-calc. [Page 77]
  • Figure 4.9.- Determination of Al2Cu and Al5Mg8Cu2Si6 start point and area. [Page 78]
  • Figure 4.10.- DTA solidification of Al Si9 Cu3 + 0.15% nano TiB2 sample. [Page 79]
  • Figure 4.11.- DTA solidification of Al Si9 sample. [Page 80]
  • Figure 4.12.- DTA solidification of 0.2% SHS-TiB2. [Page 81]
  • Figure 4.13.- DTA solidification of 0.2% commercialTiB2 briquette. [Page 81]
  • Figure 4.14.- DTA solidification of 0.1% of gamma Al2O3 briquette. [Page 84]
  • Figure 4.15.- DTA solidification of 0.17% of alpha Al2O3 briquette. [Page 85]
  • Figure 4.16.- Temperature evolution graphic. [Page 90]
  • Figure 4.17.- Recalescence comparison between samples. [Page 91]
  • Figure 4.18.- Modification comparison between samples. [Page 92]
  • Figure 4.19.- Al Si9 Cu3 alloy TP1 essay OM macrograph analysis. [Page 95]
  • Fig. 4.20.: Al Si 9 Cu3 OM micrographs. [Page 96]
  • Figure 4.21.- Al Si9 Cu3 typical SEM micrographs. [Page 96]
  • Figure 4.22.- SHS-TiB2 reinforced alloy TP1 essay OM macrograph analysis. [Page 97]
  • Fig. 4.23: OM Study of grain and precipitates in the central and peripheral areas. [Page 98]
  • Fig. 4.24.: SEM study of SHS-TiB2 reinforced alloy. [Page 99]
  • Figure 4.25.- Phase determination in SHS-TiB2 reinforced alloy by EDS and SEM. [Page 100]
  • Figure 4.26.- 0.1 wt.% γ-Al2O3 reinforced alloy TP1 essay OM macrograph analysis. [Page 101]
  • Figures 4.27.: OM Study of grain and precipitates in the central and peripheral areas. [Page 102]
  • Figure 4.28.- Phase determination in γ-Al2O3 reinforced alloy by EDS and SEM. [Page 102]
  • Figures 4.29. A,B,C,D and E.- Al2O3 particles detection by EDS and SEM. [Page 103]
  • Figures 4.30. A,B and C.- Al2O3 particles detection by EDS and SEM. [Page 105]
  • Figures 4.31.- Determination of peripheral Al dendrite composition by WDS. [Page 106]
  • Figures 4.32.- Determination of central Al dendrite composition by WDS. [Page 107]
  • Figures 4.33. A and B shows typical microstructure of the matrix taken into the center of the sample where acicular grains are found in two areas. [Page 108]
  • Figure 4.33.- A and B : TEM micrograph of typical microstructure of sample in the center of the foundry sample namely acicular grain zone. Each TEM micrograph (bright field image is associated with 4 EDS corresponding maps (Al, Cu, Si and Fe)). [Page 109]
  • Figure 4.34.- TEM micrograph of typical microstructure of sample in the edge of the foundry sample. [Page 110]
  • Figures 4.35. A) and a B) show typical microstructure of the matrix taken into the peripheral area of sample, where small grain zones are found. Each of the bright field micrograph is associated with EDS maps in order to analyze the distribution of the Al, Cu, Si and Fe elements within the TEM analysis zone. [Page 111]
  • Figure 4.35. A) and B).- TEM micrograph of typical microstructure of sample in the edge of the foundry sample namely small grain zone. Each TEM micrograph (bright field image is associated with 4 EDS corresponding maps (Al, Cu, Si and Fe)). [Page 112]
  • Figure 4.36.- Acicular dendrite zone detail in the center of a reinforced alloy. [Page 114]
  • Figure 4.37.- Secondary dendrite arm spacing determination. [Page 114]
  • Figures 4.38.- Secondary dendrite arm spacing determination. [Page 115]
  • Figure 4.39.: Comparative diagram between SDAS and IACS. [Page 120]
  • Figure 5.1: UTS at room temperature for reinforced and base Al Si9 Cu alloys. [Page 130]
  • Fig. 5.2: YS at room temperature for reinforced and base Al Si9 Cu alloys. [Page 131]
  • Fig. 5.3 Elongation at room temperature for reinforced and base Al Si9 Cu alloys. [Page 131]
  • Fig. 5.4: UTS at 200ºC for reinforced and base Al Si9 Cu alloys. [Page 133]
  • Fig. 5.5: YS at 200ºC for reinforced and base Al Si9 Cu alloys. [Page 133]
  • Fig. 5.6 Elongation at 200ºC for reinforced and base Al Si9 Cu alloys. [Page 134]
  • Figure 5.7: Fracture analysis of base alloy. [Page 136]
  • Figure 5.8: Fracture analysis of 0.02% SHS TiB2 reinforced alloy. [Page 136]
  • Figure 5.9: Fracture analysis of 0.1% Al2O3 gamma alumina reinforced alloy. [Page 137]

7. Conclusion:

Summary of key findings:

  • Nano-sized TiB2 and Al2O3 particles act as grain refiners in Al-Si9-Cu3-Fe1 alloys, modifying the solidification behavior and microstructure. [Page 142]
  • TiB2 has a more potent grain refining effect than Al2O3. [Page 142]
  • Nanoparticles reduce porosity size and quantity, with Al2O3 being more effective than TiB2. [Page 142]
  • The addition of nanoparticles generally improves the ultimate tensile strength (UTS) and elongation, especially at room temperature. [Page 143]
  • The yield strength (YS) is slightly reduced with nanoparticle addition at room temperature but increases at 200°C. [Page 143]
  • The electrical conductivity decreases with nanoparticle addition. [Page 142]

Summary of research results. Academic significance of the research, practical implications of the research

  • The addition of nanoparticles in the Al-Si alloys changes the solidification curves, promoting a better nucleation. [Page 122]
  • TiB2 particles have a great influence in the solidification and in the obtained microstructure of the aluminium alloys. [Page 3]
  • The addition of grain refiners in the Al Si9 Cu3 Fe1 as Al Ti5 B1, Al Ti3 B1 and Al Ti C have been reported [Boo 02] to decrease the internal porosity, with an average lower porosity size and with a better distribution of porosity in the part. [Page 4]
  • The microstructure and composition of the reinforced alloys has been thoroughly studied through Optical Microscopy, Scanning Electronic Microscopy (SEM), Transmission Electronic Microscopy (TEM) and Atomic Force microscopy (AFM). [Page 5]
  • The thermal and mechanical characterization has been carried out with samples obtained with the DC and HPDC process. [Page 5]
  • The experimental results have been compared with the models employed for calculating mechanical and thermal properties of materials reinforced with ceramic particles and to check the expected improvement in the alloy properties. [Page 5]

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9. Copyright:

  • This material is a paper by "Iban Vicario Gomez": Based on "Influence of Alumina (Al2O3) and Titanium Diboride (TiB2) nanoparticulates on the microstructure and properties of Al Si9 Cu3 Fe1 alloys for high pressure die casting applications.".
  • Source of paper: tel-00670402, https://tel.archives-ouvertes.fr/tel-00670402

This material was created to introduce the above paper, and unauthorized use for commercial purposes is prohibited. Copyright © 2025 CASTMAN. All rights reserved.

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