xxviii
List of Figures
(0.5, 0.20) near the layered boundary. d is a sample dispensed at
(0.5, 0.05). Right: XRD scans of the three samples in the region
near 44
◦ ..................................................................
91
Fig. 7.1
The pseudo-ternary phase diagrams obtained for the
Li–Ni–Mn–O system for combinatorial samples obtained by
quenching (a), and slow cooling (b). Red lines represent
boundaries to single-phase regions, green dashed lines are
tie-lines, red dashed lines are tie-lines bounding three-phase
regions and the blue dotted line is the phase transition between
cubic and layered rocksalt structures. There is a red tie-line
joining R and N, however the two-phase region is so small that it
cannot be distinguished from the layered boundary on the scale
shown here. Points S, M, N and R refer to the corners of the
three-phase regions and move with synthesis conditions. Points
A 7 and B 7 are two compositions referred to in the text .............
96
Fig. 7.2
X-ray diffraction (XRD) patterns obtained for bulk sample A 7 in
the Li–Mn–Ni oxide system heated to 800
◦ C. Composition A 7 is
indicated in Fig. 7.1. The right frame focuses on the XRD peaks
near 44
◦ where the four phases have one peak each. The red
dashed lines represent the positions of the N, R, S and M peaks
when slow cooled after heating in oxygen. SC denotes samples
slow cooled at 1
◦ C/min, Q stands for quenching on steel while Q
LN2 refers to quenching in liquid nitrogen, and SC/Q indicates a
slow cooled sample that was reheated to 800
◦ C and quenched.
Q/650 A and Q/750 A were quenched samples that were annealed
at 650
◦ C and 750
◦ C respectively for 5 h before quenching back
to room temperature ....................................................
98
Fig. 7.3
X-ray diffraction (XRD) scans of samples made at compositions
A 7 ’ and B 7 , indicated in Table 7.1. An expanded view of the peaks
near 44
◦ is included in the right panel. Q indicates quenched
while SC refers to slow cooling (1
◦ C/min) and SC/Q denotes a
slow cooled sample after being reheated to 800
◦ C and quenched
98
Fig. 7.4
The single-phase boundaries obtained in this study for quenched
combinatorial samples heated in oxygen (solid red lines). The
points were obtained by visual inspection of XRD scans of bulk
samples synthesized in air; the open circles represent multi-phase
samples for both quenched and regular cooled conditions, the
closed circles are single-phase for both, and the x symbols
correspond to single-phase quenched samples that phase
separates during regular cooling. The blue solid line is a rough
estimate of the boundary in air for quenched samples based on
these data points, while the blue dashed line is for regular
cooling. Further work to completely determine the phase
boundaries in air is currently being done by Aaron Rowe..........
99
List of Figures
(0.5, 0.20) near the layered boundary. d is a sample dispensed at
(0.5, 0.05). Right: XRD scans of the three samples in the region
near 44
◦ ..................................................................
91
Fig. 7.1
The pseudo-ternary phase diagrams obtained for the
Li–Ni–Mn–O system for combinatorial samples obtained by
quenching (a), and slow cooling (b). Red lines represent
boundaries to single-phase regions, green dashed lines are
tie-lines, red dashed lines are tie-lines bounding three-phase
regions and the blue dotted line is the phase transition between
cubic and layered rocksalt structures. There is a red tie-line
joining R and N, however the two-phase region is so small that it
cannot be distinguished from the layered boundary on the scale
shown here. Points S, M, N and R refer to the corners of the
three-phase regions and move with synthesis conditions. Points
A 7 and B 7 are two compositions referred to in the text .............
96
Fig. 7.2
X-ray diffraction (XRD) patterns obtained for bulk sample A 7 in
the Li–Mn–Ni oxide system heated to 800
◦ C. Composition A 7 is
indicated in Fig. 7.1. The right frame focuses on the XRD peaks
near 44
◦ where the four phases have one peak each. The red
dashed lines represent the positions of the N, R, S and M peaks
when slow cooled after heating in oxygen. SC denotes samples
slow cooled at 1
◦ C/min, Q stands for quenching on steel while Q
LN2 refers to quenching in liquid nitrogen, and SC/Q indicates a
slow cooled sample that was reheated to 800
◦ C and quenched.
Q/650 A and Q/750 A were quenched samples that were annealed
at 650
◦ C and 750
◦ C respectively for 5 h before quenching back
to room temperature ....................................................
98
Fig. 7.3
X-ray diffraction (XRD) scans of samples made at compositions
A 7 ’ and B 7 , indicated in Table 7.1. An expanded view of the peaks
near 44
◦ is included in the right panel. Q indicates quenched
while SC refers to slow cooling (1
◦ C/min) and SC/Q denotes a
slow cooled sample after being reheated to 800
◦ C and quenched
98
Fig. 7.4
The single-phase boundaries obtained in this study for quenched
combinatorial samples heated in oxygen (solid red lines). The
points were obtained by visual inspection of XRD scans of bulk
samples synthesized in air; the open circles represent multi-phase
samples for both quenched and regular cooled conditions, the
closed circles are single-phase for both, and the x symbols
correspond to single-phase quenched samples that phase
separates during regular cooling. The blue solid line is a rough
estimate of the boundary in air for quenched samples based on
these data points, while the blue dashed line is for regular
cooling. Further work to completely determine the phase
boundaries in air is currently being done by Aaron Rowe..........
99