Microstructural Engineering of Titanium-Cellulose Nanocrystals Alloys via Mechanical Alloying and Powder Processing

• Main Author: Angle, Jonathan Willis
• Other Authors: Materials Science and Engineering
• Format: Others
• Language: en_US
• Published: Virginia Tech 2019
• Subjects: Titanium; Metal Matrix Composites; Cellulose Nanocrystals; Particulate Reinforcement; Mechanical Alloying
• Online Access: http://hdl.handle.net/10919/87473

Titanium been used industrially for nearly a century. Ever since it was first reduced to its elemental form, concerted efforts have been made to improve the material and to reduce the cost of production. In this thesis, titanium is mechanically alloyed with cellulose nanocrystals followed by powder consolidation and sintering to form a solid titanium metal matrix composite. Cellulose nanocrystals (CNCs) were chosen as the particle reinforcement as they are a widely abundant and natural material. Additionally, the nanocrystals can be derived from waste materials such as pistachio shells. This offers a unique advantage to act as a green process to enhance the mechanical properties of the titanium as well as to reduce to cost of production. Vibrational milling using a SPEX 8000M mill was used to mechanically alloy titanium powder with varying concentrations of CNCs. Additionally, the milling time was varied. This process showed that varying the concentrations of CNCs between 0.5% - 2% by weight did not noticeably alter the microstructural or mechanical properties of the materials. Conversely, changing the milling time from 0.5 hours to 5 hours proved to greatly alter the microstructural and mechanical properties of the titanium matrix metal composites. Further increasing the milling time to 10 and 25 hours caused the materials to become exceedingly brittle thus, the majority of experiments focused on samples milled between 0.5 hours and 5 hours. The hardness values for the Ti-1%CNC materials increased from 325-450-600-800 for the samples milled for 0.5, 1, 2, and 5 hours respectively. The other concentrations used were found to yield similar values and trends. SEM micrographs showed that small precipitates had formed within the grains except materials milled at 5 hours, which showed the production of very coarse particles at the grain boundaries. Similarly, an attrition mill was used to mechanically alloy titanium with varying CNC concentrations. Milling time was also varied. The powders were consolidated, sintered and characterized. It was found that increasing CNC content at low milling times caused a reduction in hardness. The X-ray diffractograms also showed a trend in that the diffraction patterns shifted to the lower angle with increasing CNC concentration, thereby suggesting that the increase in CNC content facilitated the removal of oxygen atoms housed within the interstitial sites. The oxygen was observed to diffuse and precipitate platelet titanium dioxide particles. These particles were found to be located within the titanium grains and coarsened with milling time. Generally, increasing the milling time to 15 hours was found precipitate particles at the grain boundaries as well as to excessively dissolve oxygen into the titanium lattice leading to embrittlement. The materials milled for 5 hours showed the best increase in strength while maintaining good ductility. === Master of Science === Titanium has only been used industrially since the early 1940’s thanks in large to the modern advances to reduce titanium ore to its elemental state. Titanium gained much interest as a structural material because of its corrosion resistance and its exceptional strength for a lightweight metal, making the material ideal for medical and aerospace applications. Pure titanium was found to be soft and had poor wear resistance, therefore, efforts were made to create titanium alloys which mitigated these weaknesses. Often titanium is alloyed with costly and toxic elements to enhance its strength properties, making it dangerous to use in the medical field. One way to enhance the strength properties of titanium without the addition of these harmful alloying elements is to create a titanium composite by adding strong inert particles to a titanium matrix. One method to create titanium metal matrix composites is to violently mix titanium powder with the reinforcement material, through a process called mechanically alloying. Following the mixing process the powder is then compacted and heated to form a solid part through a process called sintering. While these powder processing methods are known and viable for forming titanium metal matrix composites, some of the reinforcement materials can be expensive. In this thesis, cellulose nanocrystals (CNCs) will be added as reinforcement to titanium by means of two mechanical alloying processes, vibratory milling (shaking) and attrition milling (stirring). CNCs can be derived from plant matter which is widely abundant and inexpensive. The viability of CNCs to be used as a reinforcement material, as well as the mechanical alloying processes were investigated to determine the effect on the titanium strength properties. The powder processing steps were found to cause the CNCs to react with the surrounding titanium matrix which caused beneficial oxides to form as the reinforcement materials. In general, it was found that vibratory milling caused the final titanium metal matrix composite to be hard and brittle. Attrition milling was found to be more favorable as some materials were observed to be strong yet ductile.