TY  - JOUR
T1  - Effects of in-situ formed TiB2 Phase on Mechanical Properties of Spark Plasma Sintered Boron Carbide
TT  - In-situ olarak oluşmuş TiB2 Fazının Spark Plazma Sinterleme ile Üretilmiş Bor Karbürün Mekanik Özellikleri Üzerindeki Etkileri
AU  - Başkut, Sinem
AU  - Yalama, Name
AU  - Turan, Servet
PY  - 2025
DA  - September
Y2  - 2025
DO  - 10.29109/gujsc.1699270
JF  - Gazi Üniversitesi Fen Bilimleri Dergisi Part C: Tasarım ve Teknoloji
JO  - GUJS Part C
PB  - Gazi Üniversitesi
WT  - DergiPark
SN  - 2147-9526
SP  - 1184
EP  - 1194
VL  - 13
IS  - 3
LA  - en
AB  - Due to their exceptional properties, B4C ceramics are favored in a wide range of application areas, including defense and ballistic protection, coating, aerospace, and high temperature electronic devices. However, its use will increase if its low fracture toughness and poor sinterability are improved. In this study, the effects of TiO2 as a sintering additive on B4C's density and mechanical properties were examined, along with the identification of the in-situ second phase that is likely to form during sintering with SPS. To achieve this, 5, 10, 15, and 20 wt. % TiO2 were added to B4C. The in-situ TiB2 phase was formed as a result of the reactions between B4C and TiO2 during sintering, according to XRD analyses performed on SPS-sintered samples. The release of CO gases due to reactions between TiO2 and B4C during sintering caused a slight decrease in the relative density of the B4C matrix as the TiO2 content increased. Density measurements and BSE-SEM images supported each other. The fracture toughness of the B₄C matrix improved by approximately 6, 43, 51, and 57 % with the addition of 5, 10, 15, and 20 wt.% TiO2, respectively. This enhancement is attributed to crack deflection, bridging, and blocking toughening mechanisms facilitated by the in-situ formed TiB2 phase.
KW  - TiO2
KW  - B4C
KW  - TiB2
KW  - Fracture Toughness
KW  - SPS
N2  - Due to their exceptional properties, B4C ceramics are favored in a wide range of application areas, including defense and ballistic protection, coating, aerospace, and high temperature electronic devices. However, its use will increase if its low fracture toughness and poor sinterability are improved. In this study, the effects of TiO2 as a sintering additive on B4C's density and mechanical properties were examined, along with the identification of the in-situ second phase that is likely to form during sintering with SPS. To achieve this, 5, 10, 15, and 20 wt. % TiO2 were added to B4C. The in-situ TiB2 phase was formed as a result of the reactions between B4C and TiO2 during sintering, according to XRD analyses performed on SPS-sintered samples. The release of CO gases due to reactions between TiO2 and B4C during sintering caused a slight decrease in the relative density of the B4C matrix as the TiO2 content increased. Density measurements and BSE-SEM images supported each other. The fracture toughness of the B₄C matrix improved by approximately 6, 43, 51, and 57 % with the addition of 5, 10, 15, and 20 wt.% TiO2, respectively. This enhancement is attributed to crack deflection, bridging, and blocking toughening mechanisms facilitated by the in-situ formed TiB2 phase.
CR  - Domnich V, Reynaud S, Haber RA, Chhowalla M. Boron carbide: structure, properties, and stability under stress. Journal of the American Ceramic Society. 94; 2011: 3605–3628.
CR  - Zhu Y, Cheng H, Wang Y, An R. Effects of carbon and silicon on microstructure and mechanical properties of pressureless sintered B4C/TiB2 composites. Journal of Alloys and Compounds. 772; 2019: 537–545.
CR  - Shi L, Gu Y, Chen L, Qian Y, Yang Z, Ma J. A low temperature synthesis of crystalline B4C ultrafine powders, Solid State Communication. 128; 2003: 5–7.
CR  - Thevenot F. Sintering of Boron Carbide and Boron Carbide-silicon Carbide Two-phase Materials and Their Properties. Journal of Nuclear Materials. 152; 1988: 154–162.
CR  - Rafi-ud-din GH et al. Ethylene Glycol Assisted Low-Temperature Synthesis of Boron Carbide Powder from Borate Citrate Precursors, Journal of Asian Ceramic Society. 2: 3; 2014: 268–274.
CR  - Liu L et al. Sintering Dense Boron Carbide Without Grain Growth under High Pressure, Journal of the American Ceramic Society. 101:3; 2018:1289–1297.
CR  - Tuffe S, Dubois J, Barbier G. Densification, Microstructure and Mechanical Properties of TiB2-B4C Based Composites. International Journal of Refractory Metals & Hard Materials. 14; 1996: 305–310.
CR  - Hwang C et al. Small Amount TiB2 Addition into B4C through Sputter Deposition and Hot Pressing. Journal of the American Ceramic Society. 102: 8; 2019: 4421–4426.
CR  - Khajehzadeha M, Ehsania N, Baharvandia RH, Abdollahia A, Bahaaddini M, Tamadonb A. Thermodynamical evaluation, microstructural characterization and mechanical properties of B4C–TiB2 nanocomposite produced by in-situ reaction of Nano-TiO2. Ceramics International. 46; 2020: 26970–26984.
CR  - Zhang W, Yamashita S, Kita H. Progress in pressureless sintering of boron carbide ceramics–a review. Advanced in Applied Ceramic. 118: 4; 2019: 222-239.
CR  - Sedlák R, Kovalčíková A, Múdra E,  Rutkowski P, Dubiel A,  Girman V, Bystrický R,  Dusza J. Boron carbide/graphene platelet ceramics with improved fracture toughness and electrical conductivity. Journal of the European Ceramic Society 37: 12; 2017: 3773-3780.
CR  - Mashhadi M, Nassaj ET, Sglavo VM. Pressureless sintering of boron carbide. Ceramics International. 36: 1; 2010: 151–159.
CR  - Kelvin Y, Xie M, Toksoy F, Kuwelkar K, Zhang B, Krogstad JA, Haber RA, Hemker KJ. Effect of Alumina on the Structure and Mechanical Properties of Spark Plasma Sintered Boron Carbide. Journal of the American Ceramic Society 97: 11; 2014: 3710–3718.
CR  - Goldstein A, Geffen Y, Goldenberg A. Boron Carbide–Zirconium Boride In Situ Composites by the Reactive Pressureless Sintering of Boron Carbide–Zirconia Mixtures. Journal of the American Ceramic Society 84: 3; 2001: 642–644.
CR  - Yao W, Yan J, Li X, Chen P, Zhu Y, Zhu B. In Situ ZrB2 Formation in B4C Ceramics and Its Strengthening Mechanism on Mechanical Properties. Materials. 15; 2022 7961.
CR  - Perevislov SN, Lysenkov AS, Vikhman SV. Effect of Si Additions on the Microstructure and Mechanical Properties of Hot-Pressed B4C. Inorganic Materials. 53: 4; 2017: 376–380.
CR  - Liua G, Chenb S, Zhaoc Y, Fua Y, Wang Y. Effect of Ti and its compounds on the mechanical properties and microstructure of B4C ceramics fabricated via pressureless sintering. Ceramics International, 47: 10;  2021: 13756-13761.
CR  - Şahin FÇ, Mansoor M, Cengiz M, Apak B, Yanmaz L, Balazsi K, Fogarassy Z, Derin B, Göller G, Yücel O. B4C Composites with a TiB2-C Core–Shell Microstructure Produced by Self-Propagating High-Temperature Synthesis-Assisted Spark Plasma Sintering. The Journal of Physical Chemistry C. 126: 47; 2022: 20114-20126. 
Twardowska A, Kowalski M. The Microstructure, Mechanical, and Friction-Wear Properties of Boron Carbide-Based Composites with TiB2 and SiC Formed In Situ by Reactive Spark Plasma Sintering. Materials, 17; 2024: 2379.
CR  - Wang S, Yuan Y, Hanc W, Yin Z. Microstructure and mechanical properties of B4C-TiB2 composite ceramic fabricated by reactive spark plasma sintering. International Journal of Refractory Metals and Hard Materials. 92; 2020: 105307.
CR  - Rangel ER. Fracture Toughness Determinations by Means of Indentation Fracture, Nanocomposites with Unique Properties and Applications in Medicine and Industry. InTechOpen. 2011: ISBN:978-953-307-351-4.
Kakazey M, Vlasova M, Gonzalez-Rodriguez JG, Dominguez-Patino M, Leder R. X-ray and EPR study of reactions between B4C and TiO2, Materials Science Engineering A. 418; 2006: 111-114.
CR  - Levin L, Frage N, Dariel MP. The effect of Ti and TiO2 additions on the pressureless sintering of B4C. Metallurgical and Materials Transactions A, 30;1999: 3201-3210.
CR  - Yang LK,  Shen P,  Guo R-F, Jiang Q-C.  The role of TiO2 incorporation in the preparation of B4C/Al laminated composites with high strength and Toughness. Ceramics International. 44:13; 2018: 15219-15227.
CR  - Asghar Z, Aziz T, Khan AR, Shah A, Waqas H, Ali F, Rasul HT, Khan MF. High-Hardness High-Fracture-Toughness B4C-TiB2 Composite Produced by Reactive Hot Pressing.  Journal of Materials Engineering and Performance. 32; 2023: 7225–7233.
CR  - He Q et al. Microstructures and Mechanical Properties of B4C-TiB2-SiC Composites Fabricated by Ball Milling and Hot Pressing. Journal of the Eıropean Ceramic Society. 38:7; 2018: 2832–2840.
CR  - Sigl LS, Kleebe HJ. Microcracking in B4C-TiB2 Composites. Journal of American Ceramic Society. 78: 9; 1995: 2374–2380.
CR  - Wang W, Lian J, Ru H. Pressureless sintered SiC matrix toughened by in situ synthesized TiB2: process conditions and fracture Toughness. Ceramics International. 38; 2012: 2079-2085.
UR  - https://doi.org/10.29109/gujsc.1699270
L1  - https://dergipark.org.tr/tr/download/article-file/4869976
ER  -